CN115738348A - Anti-blocking cooling crystallizer, cooling crystallization method and application thereof - Google Patents

Anti-blocking cooling crystallizer, cooling crystallization method and application thereof Download PDF

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Publication number
CN115738348A
CN115738348A CN202211425239.4A CN202211425239A CN115738348A CN 115738348 A CN115738348 A CN 115738348A CN 202211425239 A CN202211425239 A CN 202211425239A CN 115738348 A CN115738348 A CN 115738348A
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cooling
wall
shell
crystallizer
gas
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陈思明
段东平
李燕江
刘艳
胡凯
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Institute of Process Engineering of CAS
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Institute of Process Engineering of CAS
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Abstract

The invention provides an anti-blocking cooling crystallizer, a cooling crystallization method and application thereof. When the cold gas product enters from the air inlet and contacts with the air wall, the kinetic energy of the protective air flow improves the heat diffusion efficiency of the cold gas product, improves the cooling speed, effectively prevents the direct contact of the gas product and the cooling wall, and prevents the cooler from being blocked due to the explosion and nucleation of a cold solidified body on the surface of the cooling wall; the cooling medium is sprayed from the nozzle, so that the cooling temperature can be accurately regulated and controlled, and the cooling medium can be used as a crystal nucleus to promote crystallization, so that the supercooling phenomenon is avoided; the synergistic effect of the two structures can ensure that the gaseous product can be effectively cooled and effectively prevent the equipment from being blocked in the cooling process.

Description

Anti-blocking cooling crystallizer, cooling crystallization method and application thereof
Technical Field
The invention belongs to the field of cooling crystallization equipment, and relates to an anti-blocking cooling crystallizer, a cooling crystallization method and application thereof.
Background
With the development of science and technology, the demand of people for electric power is continuously increasing. In the power industry of China, the proportion of thermal power is obviously higher than that of hydraulic power and renewable power, the proportion of coal power in thermal power is high, and the trend still keeps for a long time. Coal power often produces a large amount of waste fly ash, and the stacking not only seriously occupies land resources, but also has larger hidden danger of environmental pollution, so that the fly ash needs to be comprehensively treated and recycled.
The fly ash contains a large amount of elements such as aluminum, iron, silicon and the like, can be effectively applied to the fields of electrolytic aluminum production, soil improvement agents and the like through treatment, can also contain heavy metal elements such as chromium, lead, nickel and the like and rare metal elements such as gallium, niobium and the like according to different sources of the coal ash, and has recycling value. At present, the utilization of the fly ash in China still mainly aims at producing low-economic added-value products such as cement, floor tiles and the like, the high-value utilization efficiency of valuable components is low, so that the serious waste of valuable elements is caused, the sustainable development of the resource utilization of the fly ash is not facilitated, and therefore, the extraction and separation technology of the valuable components of the fly ash is continuously developed and improved to achieve the aim and the requirement of high-value recovery.
At present, methods for extracting valuable components of fly ash mainly comprise an acid leaching method, an alkali leaching method, a chlorination method and the like, wherein the chlorination method is concerned by people due to simple process, high treatment efficiency and obviously reduced slag yield compared with other methods. However, the chlorination process has problems: the obtained gaseous chlorination product is easy to explode to nucleate and crystallize on the surface of a cooling wall or a cooling coil, so that the cooling crystallizer is blocked; in addition, because the solidification temperature intervals of gaseous products such as ferric chloride, aluminum chloride, silicon chloride and the like are not very different, the adoption of a conventional cooling crystallizer can cause a local supercooling phenomenon, thereby causing the reduction of product purity.
At present, there are some reports on the apparatus and method for cooling and crystallizing gas product or product to be cooled in gaseous state:
CN216986963U discloses a thin-wall trap for continuously trapping gas-phase pyromellitic dianhydride, which is mainly suitable for trapping pyromellitic dianhydride in the gas at the outlet of a reactor in a pyromellitic dianhydride catalyst pilot-scale evaluation device. The fixed knocking rod is arranged on the outer wall of the trap box body and can knock materials on the box wall, and the movable knocking rod is arranged in the box body and is mainly used for removing the homogeneous anhydride materials attached to the trap baffle plates.
CN215741889U has provided a recovery of cyanuric chloride crystallization tail gas and has recycled device, including the gas generator who communicates in proper order, the one-level crystallizer, cooling crystallizer and dust collector, gas generator includes first feed inlet and first gas outlet, the one-level crystallizer communicates with gas generator through first gas outlet, one-level crystallizer and dust collector have first discharge gate and second discharge gate respectively, dust collector still has the second gas outlet, still include the diaphragm compressor with second gas outlet intercommunication, communicate the first passageway of gas generator and diaphragm compressor. The device can solve the problem of waste of resources such as chlorine, chlorocyanogen, cyanuric chloride and the like in the related technology.
CN113860338A discloses a preparation and purification device for high-purity anhydrous beryllium chloride, the gas path system of which is communicated with a chlorination reactor through a main gas inlet path, the chlorination reactor is connected with a condenser and is communicated with a multi-stage cyclone separator through a pipeline; the multistage cyclone separator is communicated with the tail gas absorption system through a pipeline, the device can remove impurities such as silicon, aluminum and iron in the raw materials, and high-purity anhydrous beryllium chloride solid is obtained in a receiver at the bottom end of the condenser.
CN113651725A discloses a system and a method for preparing dicyandiamide by reusing melamine tail gas, wherein a part of the melamine tail gas is introduced into a crystallizer through a cold air compressor, a part of the melamine tail gas is introduced into a reactor, and simultaneously a small amount of carbon dioxide is introduced to react to obtain a dicyandiamide gas, the dicyandiamide gas containing solid impurities is filtered by a first filter and then polymerized in a polymerization reactor to obtain a dicyandiamide gas, the solid impurities contained in the dicyandiamide gas are filtered by a second filter and then enter the crystallizer with the melamine tail gas as process cold air to be cooled and crystallized, and then a dicyandiamide solid is collected in a trap, a part of the gas is reused as process gas, and a part of the gas is treated and reused as process tail gas.
The device and the method can meet the problems of cooling and separating gas products to a certain extent, and also relate to the temperature control of the condensation process by using the process gas as a cooling medium, but the conventional cooling device is still adopted in the patent, so that an effective solution is not provided for the problems of crystallization blockage and crystallization temperature control.
Disclosure of Invention
In view of the problems in the prior art, an object of the present invention is to provide an anti-clogging cooling crystallizer, a cooling crystallization method and an application thereof, wherein a housing of the anti-clogging cooling crystallizer is provided with an air inlet, an air outlet, a cooling medium nozzle and a shielding gas inlet, a cooling wall interlayer connected to the shielding gas inlet is arranged inside the cooling crystallizer, the cooling wall interlayer comprises a first cooling wall facing the air inlet, and the first cooling wall is provided with fine holes arranged in an array for forming an air wall facing the air inlet in the housing by the shielding gas. When the product to be cooled enters from the air inlet and contacts with the air wall, the heat transfer efficiency of cooling can be improved, the cooling speed is improved, meanwhile, the product to be cooled is effectively prevented from directly contacting with the cooling wall, and the cooler is prevented from being blocked due to the explosion nucleation of a cold solidification body on the surface of the cooling wall; the cooling medium is sprayed from the nozzle, so that the cooling temperature can be accurately regulated and controlled, and the cooling medium can be used as a crystal nucleus to promote crystallization, so that supercooling is avoided; the synergistic effect of the two can ensure that the gaseous product can be efficiently cooled, and simultaneously, the equipment blockage in the cooling process can be effectively prevented.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides an anti-clogging cooling crystallizer, which comprises a shell, wherein the upper part of the shell is provided with an air inlet, an air outlet, a cooling medium nozzle and a protective gas inlet, and the bottom of the shell is provided with a discharge hole;
a cooling wall interlayer is arranged in the shell, the cooling wall interlayer is a semi-sealing structure with a cavity, and the cavity is opened at one side of the cooling wall interlayer and is connected with the protective gas inlet; the cooling wall sandwich layer comprises a first cooling wall facing the air inlet and a second cooling wall opposite to the first cooling wall and facing away from the air inlet; the first cooling wall is provided with fine holes which are arranged in an array mode, and the fine holes are used for forming air walls facing the air inlet in the shell through the protective air in the cavity.
The invention provides a cooling crystallizer with high-efficiency cooling crystallization and blockage prevention, wherein a cooling wall interlayer is arranged in the cooling crystallizer, so that protective gas passes through fine holes arrayed on the cooling wall interlayer to generate a protective gas wall facing a gas inlet of a product to be cooled in a shell, and the product to be cooled is separated from the cooling wall, so that the heat transfer efficiency of the cooling process of a gas product can be improved, the temperature reduction of the gas product is accelerated, meanwhile, the direct contact of the gas product and the cooling wall can be effectively prevented, and the blockage of a cooler caused by the explosion nucleation of a cold solidified body on the surface of the cooling wall is prevented; according to the invention, the cooling medium with a certain temperature is sprayed from the cooling medium spray opening, so that the precise regulation and control of the cooling temperature can be realized, the cooling medium can be any one of solid, liquid or gas state or the combination of at least two of the solid, liquid or gas state, the cooling medium can be used as a crystal nucleus to promote the crystallization of a gaseous product and avoid the generation of a supercooling phenomenon, and the gas product can be ensured to realize an efficient cooling and crystallization process in the cooler provided by the invention through the synergistic effect, and the equipment blockage in the cooling process can be effectively prevented.
Furthermore, the invention can adjust the position between the interlayer of the cooling wall and the air inlet, the pore diameter of the fine pores arranged in an array, the total area of the pores, the horizontal included angle of the pores and other device structure parameters according to the type of the to-be-cooled gaseous product to be processed, and adjust and match the spraying speed and the temperature of the specific to-be-cooled gaseous product, the cooling medium and the protective gas, so that the effects of efficient cooling crystallization and blockage prevention are optimal, and the invention is suitable for different cooling crystallization processes.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
As a preferable technical solution of the present invention, the air inlet is provided on a side wall of the casing, and the cooling medium nozzle is provided on a top surface of the casing and between the air inlet and the first cooling wall.
Preferably, the air outlet is provided on a side wall of the other side of the housing opposite to the air inlet.
When the product to be cooled is introduced into the anti-clogging cooling crystallizer from the air inlet on the side wall, the arrangement of the cooling wall interlayer changes the flow of the product to be cooled in the inner part, so that the product to be cooled enters the cavity below the anti-clogging cooling crystallizer, passes through the space between the second cooling wall of the cooling wall interlayer and the air outlet, and is discharged out of the anti-clogging cooling crystallizer from the air outlet, therefore, the product to be cooled in the inner part can be cooled at the positions such as the position near the first cooling wall surface, the position of the second cooling wall, the position of the inner wall surface of the shell where the air inlet is positioned, the position of the inner cavity wall below the shell and the like. When the cooling wall interlayer is not arranged, the gas to be cooled is directly discharged from the gas outlet after entering from the gas inlet, so that the retention time of the gas to be cooled in the cooling crystallizer is too short, and the cooling efficiency is low; therefore, the arrangement of the cooling wall interlayer can effectively improve the gas residence time, but when the to-be-cooled gaseous product is directly cooled on the cooling wall surface, the to-be-cooled gaseous product is easy to scale due to supercooling, so that the gas wall is increased by arranging the cooling wall interlayer, the aim of preventing the gas from approaching and directly contacting the cooling wall surface is fulfilled, and the purpose of prolonging the residence time is also fulfilled.
As a preferable technical solution of the present invention, the shielding gas inlet is disposed on the top surface of the housing and between the cooling medium nozzle and the gas outlet.
Preferably, the horizontal distance between the side wall of the shielding gas inlet and the side wall of the gas inlet is 30% to 70% of the horizontal distance between the side wall of the gas inlet and the side wall of the gas outlet, for example, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, or 70%, but not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
Because the cooling wall interlayer is connected to the shielding gas inlet, the horizontal distance between the shielding gas inlet and the side wall where the gas inlet is located accounts for 30% -70% of the horizontal distance between the side wall where the gas inlet is located and the side wall where the gas outlet is located, that is, the horizontal distance between the cooling wall interlayer (ignoring the width between the first cooling wall and the second cooling wall) and the side wall where the gas inlet is located accounts for 30% -70% of the horizontal distance between the side wall where the gas inlet is located and the side wall where the gas outlet is located.
As a preferable technical solution of the present invention, the pores arranged in the array on the first cooling wall are arranged in a honeycomb manner.
Preferably, the pore size of the pores arranged in the array is 0.05 to 1mm, such as 0.05mm, 0.1mm, 0.2mm, 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm or 10mm, but not limited to the recited values, and other values not recited in the above range of values are equally applicable.
Preferably, the total hole area of the fine holes arranged in the array accounts for 70% to 95% of the surface area of one side of the first cooling wall, for example, 70%, 75%, 80%, 85%, 90%, or 95%, but is not limited to the enumerated values, and other values not enumerated in the above numerical range are also applicable.
Preferably, from the inner surface of the first cooling wall close to the cavity to the outer surface far from the cavity, each of the arrayed pores is inclined towards the bottom of the housing, and the horizontal included angle of the arrayed pores is 0 ° to 20 °, such as 0 °, 2 °, 4 °, 6 °, 8 °, 10 °, 12 °, 14 °, 16 °, 18 °, or 20 °, but not limited to the enumerated values, and other non-enumerated values in the above-mentioned range of values are also applicable.
When the horizontal included angle of the fine holes arranged in an array is 0 degree, namely the fine holes arranged in an array are arranged in parallel with the horizontal plane, the fine holes are arranged according to a specific inclined direction and a specific inclined angle, and the purpose is to prevent the gas to be cooled from being separated out at the opening position of the fine holes due to overlarge flow rate, and the fine holes are blocked due to the sedimentation of part of crystals at the fine holes.
As a preferable technical scheme of the invention, the discharge port is connected with a related air blower.
Preferably, in the housing, a side wall where the air outlet is located has an inclined surface extending obliquely toward the discharge port.
In a preferred embodiment of the present invention, the material of the housing and the material of the cooling wall interlayer both include a first material and a second material.
Preferably, the first material comprises carbon steel and/or glass fiber reinforced plastic.
Preferably, the second material comprises any one or a combination of at least two of stainless steel, pure titanium, poly-tetrachloroethylene or pure nickel, typical but non-limiting examples of which include stainless steel in combination with pure titanium, stainless steel in combination with poly-tetrachloroethylene, stainless steel in combination with pure nickel, pure nickel in combination with pure titanium, pure titanium in combination with poly-tetrachloroethylene, poly-tetrachloroethylene in combination with pure nickel.
Preferably, the outer wall of the shell is made of a first material, and the inner wall of the shell is made of a second material.
Preferably, the material of the outer wall of the cooling wall interlayer is the second material, and the material of the inner wall of the cooling wall interlayer is the first material.
Since the interior of the cooling crystallizer needs to be in contact with a corrosive chlorinated gas, the inner wall of the shell and the outer wall of the cooling wall interlayer are preferably made of corrosion-resistant materials.
Preferably, heating wires and/or heat insulating layers are mounted on the outside of the housing.
In a preferred embodiment of the present invention, the cooling medium nozzle includes any one of a circular nozzle, a spiral nozzle, a hollow tapered nozzle, and a pipe nozzle.
In a second aspect, the present invention provides a cooling crystallization method, which employs the blockage-preventing cooling crystallizer of the first aspect, and comprises the following steps:
s1, injecting a cooling medium into the shell from the cooling medium nozzle; protective gas is fed into the cavity of the cooling wall interlayer through a protective gas inlet, and a gas wall facing the gas inlet is formed by the fine holes arranged in the array on the first cooling wall;
and S2, delivering the to-be-cooled gaseous product into the shell from the air inlet, contacting with a cooling medium for cooling, and discharging the obtained solid product from the discharge hole after the obtained solid product falls to the bottom of the shell for collection.
As a preferred embodiment of the present invention, the velocity of the cooling medium passing through the cooling medium nozzle is 1 to 60cm/s, for example, 1cm/s, 5cm/s, 15cm/s, 20cm/s, 25cm/s, 30cm/s, 35cm/s, 40cm/s, 45cm/s, 50cm/s, 55cm/s or 60cm/s, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
Preferably, the velocity of the shielding gas through the shielding gas inlet is in the range of 1 to 60cm/s, such as 1cm/s, 5cm/s, 15cm/s, 20cm/s, 25cm/s, 30cm/s, 35cm/s, 40cm/s, 45cm/s, 50cm/s, 55cm/s or 60cm/s, and the like, but is not limited to the recited values, and other values not recited within the above range of values are equally applicable.
Preferably, the velocity of the product in the cold gaseous state through the inlet is between 1 and 20cm/s, for example 1cm/s, 2cm/s, 4m/s, 6cm/s, 8cm/s, 10cm/s, 12cm/s, 14cm/s, 16cm/s, 18cm/s or 20cm/s, etc., but is not limited to the values listed, other values not listed in the above range of values being equally applicable.
In a third aspect, the invention provides a use of the cooling crystallization method of the second aspect in treating fly ash by a chlorination process.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) The anti-blocking cooling crystallizer provided by the invention has the advantages that the air wall is generated in the anti-blocking cooling crystallizer, so that the heat transfer efficiency of a to-be-cooled gaseous product in a cooling process can be improved, the temperature reduction rate of the to-be-cooled gaseous product is accelerated, meanwhile, the to-be-cooled gaseous product can be effectively prevented from being in direct contact with the cooling wall, and the blockage of a cooler caused by the explosion nucleation of a cold solidified body on the surface of the cooling wall is prevented; the cooling medium with a certain temperature is sprayed from the cooling medium spray opening, so that the cooling temperature can be accurately regulated, meanwhile, the cooling medium can also be used as a crystal nucleus to promote the crystallization of a gas product and avoid the generation of a supercooling phenomenon, the synergistic effect of the cooling medium and the crystal nucleus can ensure that the gas product realizes an efficient cooling crystallization process, and the equipment in the cooling process can be effectively prevented from being blocked;
(2) The structure and airflow distribution of the air wall are adjusted by changing the aperture size, the total hole area and the horizontal included angle of the holes of the first cooling wall on the cooling wall interlayer, and the interaction of the cooling wall interlayer (a shielding gas inlet) and the air inlet, the product in a cold gas state to be cooled, the cooling medium and the shielding gas in the shell is further adjusted by adjusting the position relation of the cooling wall interlayer and the air inlet speed of the shielding gas, so that the cooling crystallization and anti-blocking effects are further improved.
Drawings
FIG. 1 is a schematic view of the structure of the cooling crystallizer for preventing clogging in the embodiment 1;
in the figure: 1-shell, 2-air inlet, 3-air outlet, 4-cooling medium nozzle, 5-protective gas inlet, 6-discharge port, 7-cooling wall interlayer, 71-cavity, 72-first cooling wall, 73-fine holes arranged in array, 74-second cooling wall, 8-inclined plane and 9-air seal machine.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
This example provides an anti-clogging cooling crystallizer, whose schematic diagram is shown in fig. 1, from which it can be seen that:
the anti-blocking cooling crystallizer comprises a shell 1, wherein a gas inlet 2 is formed in the side wall of one side of the upper part of the shell 1, and a gas outlet 3 is formed in the side wall of the other side of the shell 1 opposite to the gas inlet 2; the top surface of the upper part of the shell 1 is also provided with a cooling medium nozzle 4 and a shielding gas inlet 5, and the cooling medium nozzle 4 is arranged between the gas inlet 2 and the shielding gas inlet 5; the protective gas inlet 5 is arranged between the cooling medium nozzle 4 and the gas outlet 3; the bottom of the shell 1 is provided with a discharge hole 6; the discharge port 6 is connected with a related air blower 9;
the air inlet 2, the cooling medium nozzle 4 and the shielding gas inlet 5 are respectively connected with an air inlet pipe, a cooling medium inlet pipe and a shielding gas inlet pipe, and are respectively used for conveying a to-be-cooled gaseous product, a cooling medium and shielding gas to the interior of the shell 1;
the horizontal distance between the shielding gas inlet 5 and the side wall where the gas inlet 2 is located accounts for 45% of the horizontal distance between the side wall where the gas inlet 2 is located and the side wall where the gas outlet 3 is located; in the shell 1, the side wall where the air outlet 3 is located is provided with a slope 8 which extends towards the discharge hole in an inclined manner;
a cooling wall interlayer 7 is arranged in the shell 1, and the cooling wall interlayer 7 is a semi-sealing structure with a cavity 71; the stave interlayer 7 comprises a first stave 72 facing the intake port 2 and a second stave 74 opposite the first stave 72 and facing away from the intake port 2; the top end edge of the first cooling wall 71 and the top end edge of the second cooling wall 72 are both connected to the shielding gas inlet 5, and the other edges of the first cooling wall 71 and the other edges of the second cooling wall 72 are correspondingly connected to form a seal and leave a cavity 71, namely, the cavity 71 is opened at one side of the cooling wall interlayer 7 and is connected to the shielding gas inlet 5 for the shielding gas to enter the cooling wall interlayer 7 from the shielding gas inlet 5;
the first cooling wall 72 is provided with fine holes 73 arranged in a honeycomb array manner, and the fine holes are used for forming an air wall facing the air inlet 2 in the shell 1 by the protective air in the cavity 71; the pore diameter of the fine pores 73 arranged in an array is 0.5mm; the total hole area of the fine holes 73 arranged in the array accounts for 95% of the surface area of one side of the first cooling wall 72; from the inner surface of the first cooling wall 72 close to the cavity 71 to the outer surface far away from the cavity 71, each fine hole 73 arranged in the array is inclined towards the bottom (discharge hole 6) of the shell 1, and the horizontal included angle of the fine holes 73 arranged in the array is 10 degrees;
the outer wall of the shell 1 is made of carbon steel, and the inner wall of the shell 1 is made of stainless steel; the outer wall of the cooling wall interlayer 7 is made of pure titanium, and the inner wall of the cooling wall interlayer 7 is made of glass fiber reinforced plastics; a heating wire and a heat-insulating layer are arranged outside the shell 1; the cooling medium nozzle 4 is a spiral nozzle.
Example 2
In the anti-clogging cooling crystallizer, the horizontal distance between the protective gas inlet and the side wall where the gas inlet is located accounts for 60% of the horizontal distance between the side wall where the gas inlet is located and the side wall where the gas outlet is located, and the pore diameter of the fine pores arranged in an array is 0.1mm; the total hole area of the fine holes arranged in the array accounts for 90% of the surface area of one side of the first cooling wall; from the inner surface of the first cooling wall close to the cavity to the outer surface far away from the cavity, each fine hole arranged in the array inclines towards the bottom of the shell, and the horizontal included angle of the fine holes arranged in the array is 15 degrees; except for the above, the other conditions were exactly the same as in example 1.
Example 3
In the anti-clogging cooling crystallizer, the horizontal distance between the protective gas inlet and the side wall where the gas inlet is located accounts for 50% of the horizontal distance between the side wall where the gas inlet is located and the side wall where the gas outlet is located, and the pore diameter of the fine pores arranged in an array is 0.25mm; the total pore area of the fine pores arranged in the array accounts for 92% of the surface area of one side of the first cooling wall; from the inner surface of the first cooling wall close to the cavity to the outer surface far away from the cavity, each fine hole arranged in an array is inclined towards the bottom of the shell, and the horizontal included angle of the fine holes arranged in the array is 18 degrees; except for the above, other conditions were exactly the same as in example 1.
Example 4
In the anti-clogging cooling crystallizer, the horizontal distance between the protective gas inlet and the side wall of the gas inlet accounts for 70% of the horizontal distance between the side wall of the gas inlet and the side wall of the gas outlet, and the pore diameters of the fine pores arranged in an array are 1mm; the total pore area of the fine pores arranged in the array accounts for 80% of the surface area of one side of the first cooling wall; from the inner surface of the first cooling wall close to the cavity to the outer surface far away from the cavity, each fine hole arranged in the array inclines towards the bottom of the shell, and the horizontal included angle of the fine holes arranged in the array is 5 degrees; except for the above, the other conditions were exactly the same as in example 1.
Example 5
The embodiment provides an anti-clogging cooling crystallizer, and the conditions of the anti-clogging cooling crystallizer are completely the same as those of embodiment 1 except that the horizontal distance between the shielding gas inlet and the side wall where the gas inlet is located is adjusted from 45% to 25% of the horizontal distance between the side wall where the gas inlet is located and the side wall where the gas outlet is located.
Example 6
The present embodiment provides an anti-clogging cooling crystallizer, and the conditions of the anti-clogging cooling crystallizer are completely the same as those in embodiment 1 except that the horizontal distance between the shielding gas inlet and the side wall where the gas inlet is located is adjusted from 45% to 30% of the horizontal distance between the side wall where the gas inlet is located and the side wall where the gas outlet is located.
Example 7
The present embodiment provides an anti-clogging cooling crystallizer, and the conditions of the anti-clogging cooling crystallizer are completely the same as those in embodiment 1 except that the horizontal distance between the shielding gas inlet and the side wall where the gas inlet is located is adjusted from 45% to 70% of the horizontal distance between the side wall where the gas inlet is located and the side wall where the gas outlet is located.
Example 8
The embodiment provides an anti-clogging cooling crystallizer, and the conditions of the anti-clogging cooling crystallizer are completely the same as those of embodiment 1 except that the horizontal distance between the shielding gas inlet and the side wall where the gas inlet is located is adjusted from 45% to 75% of the horizontal distance between the side wall where the gas inlet is located and the side wall where the gas outlet is located.
Example 9
This example provides an anti-clogging cooling crystallizer which is identical to that of example 1 except that the pore diameter of the fine pores arranged in the array is adjusted from 0.5mm to 0.02 mm.
Example 10
This example provides an anti-clogging cooling crystallizer, which is identical to that of example 1 except that the pore diameter of the fine pores arranged in the array is adjusted from 0.5mm to 0.05 mm.
Example 11
This example provides an anti-clogging cooling crystallizer, which is identical to that of example 1 except that the pore diameter of the fine pores arranged in the array is adjusted from 0.5mm to 1 mm.
Example 12
This example provides an anti-clogging cooling crystallizer, which is identical to that of example 1 except that the pore diameter of the fine pores arranged in the array is adjusted from 0.5mm to 1.3 mm.
Example 13
This example provides an anti-clogging cooling crystallizer which is identical to that of example 1 except that the total hole area of the fine holes arranged in the array is adjusted from 95% to 65% of the surface area of one side of the first cooling wall.
Example 14
This example provides an anti-clogging cooling crystallizer which is identical to that of example 1 except that the total hole area of the fine holes arranged in the array is adjusted from 95% to 70% of the surface area of one side of the first cooling wall.
Example 15
This example provides an anti-clogging cooling mold, which is identical to example 1 except that the total pore area of the fine pores arranged in an array is adjusted from 95% to 98% in the surface area of one side of the first cooling wall.
Example 16
In the anti-clogging cooling crystallizer, from the inner surface of the first cooling wall close to the cavity to the outer surface far away from the cavity, each fine hole arranged in an array inclines towards the top (cooling medium nozzle) of the shell, the horizontal included angle of the fine holes arranged in the array is 10 degrees, and other conditions are completely the same as those in embodiment 1.
Example 17
The embodiment provides an anti-clogging cooling crystallizer, in which the fine holes arranged in an array are parallel to a horizontal plane, that is, a horizontal included angle of the fine holes arranged in the array is adjusted from 10 ° to 0 °, and other conditions are completely the same as those in embodiment 1.
Example 18
In the anti-clogging cooling crystallizer, from the inner surface of the first cooling wall close to the cavity to the outer surface far away from the cavity, each fine hole arranged in an array inclines towards the bottom (discharge port) of the shell, the horizontal included angle of the fine holes arranged in the array is adjusted to 20 degrees, and other conditions are completely the same as those in embodiment 1.
Example 19
In the anti-clogging cooling crystallizer, from the inner surface of the first cooling wall close to the cavity to the outer surface far away from the cavity, each fine hole arranged in an array inclines towards the bottom (discharge port) of the shell, the horizontal included angle of the fine holes arranged in the array is adjusted to 30 degrees, and other conditions are completely the same as those in embodiment 1.
Example 20
The embodiment provides an anti-clogging cooling crystallizer, wherein an inclined surface obliquely extending towards the discharge port is not arranged on the side wall where the gas outlet is located in the anti-clogging cooling crystallizer, and the rest conditions are completely the same as those in embodiment 1.
Comparative example 1
This comparative example provides a cooling crystallizer in which no cooling wall interlayer is provided, and the other conditions are exactly the same as in example 1.
The method for cooling and crystallizing a product to be cooled in a blockage-preventing cooling crystallizer provided in examples 1 to 4 comprises the following steps:
s1, injecting a cooling medium with a specific temperature and a specific material state into the shell from the cooling medium nozzle; protective gas is fed into the cavity of the cooling wall interlayer through a protective gas inlet, and a gas wall facing the gas inlet is formed by the fine holes arranged in the array on the first cooling wall;
s2, sending the to-be-cooled gaseous product with the specified temperature into the shell from the air inlet, contacting with a cooling medium for cooling, allowing the obtained solid product to fall into a middle bin at the bottom of the shell for collection, and periodically discharging the formed solid product through an air seal machine.
In the method for performing the cooling crystallization by using the anti-clogging cooling crystallizer, the spraying temperature and the spraying speed of the corresponding to-be-cooled gaseous product, the cooling medium and the shielding gas are set according to the specific structural characteristics in the anti-clogging cooling crystallizer, and the parameters in all aspects interact with each other to optimize the cooling crystallization effect and the anti-clogging effect, for example, the parameter settings of the embodiments 1 to 4 respectively aiming at the cooling crystallization of different to-be-cooled gaseous products can be set according to the values recorded in the table 1.
TABLE 1
Figure BDA0003941975260000151
Figure BDA0003941975260000161
In Table 1, d Cooling wall Representing that the horizontal distance between the protective gas inlet (and the cooling wall interlayer connected with the protective gas inlet) and the side wall of the gas inlet accounts for the side wall of the gas inlet and the side wall of the gas outletA percentage of the horizontal spacing of the walls; r Hole(s) The pore diameter of the pores in the array arrangement is represented; phi is a unit of Hole(s) Representing the percentage of the total hole area of the fine holes arranged in the array to the surface area of one side of the first cooling wall; theta Hole(s) Representing the horizontal included angle of the fine holes arranged in the array; v is a cell Cooling medium Represents the velocity of the cooling medium through the cooling medium nozzle; upsilon is Protective gas Represents the velocity of the shielding gas through the shielding gas inlet; v is a cell To cool the gaseous product Representing the velocity of the gaseous product to be cooled through the inlet.
Table 2 shows the effect of cooling crystallization of examples 1 to 4 according to the values in Table 1, and the cooling crystallization test of examples 5 to 20 and comparative example 1 was carried out according to the composition of the product to be cooled in the gas state, the cooling medium, the shielding gas and the spraying speed of the product to be cooled in Table 1 corresponding to example 1, and the results are also shown in Table 2.
TABLE 2
Figure BDA0003941975260000162
Figure BDA0003941975260000171
As can be seen from table 2: d Cooling wall In relation to the effective cooling volume in the cooler, d Cooling wall Too small results in too small an effective cooling volume and thus too low cooling efficiency; and d Cooling wall If too large, the effect of the stave will be reduced. R Hole(s) And phi Hole(s) Jointly determine the anti-blocking effect of the cooling wall, R Hole(s) Too large a size results in crystals of the gas to be cooled easily accumulating in the pores and causing clogging, and R Hole(s) The pressure is too small, so that on one hand, the conveying pressure of the protective gas is too large, and the production and application are not facilitated; phi is a Hole(s) Too small a diameter tends to cause the cooling product to precipitate at the non-perforated part of the cooling wall and to clog it Hole(s) Too large results in a reduction in the structural strength of the stave. Theta.theta. Hole(s) With cooling of the product in the poresIn relation to the deposition when theta Hole(s) At negative angles, the cooled product may clog due to gravity.
The anti-blocking cooling crystallizer is provided with the cooling wall interlayer, so that the cooling efficiency is improved, direct contact between a product in a cold gas state to be cooled and the cooling wall can be effectively prevented, and the cooler is prevented from being blocked due to explosion nucleation of a cold solidified body on the surface of the cooling wall; the cooling medium is sprayed from the nozzle, so that the cooling temperature can be accurately regulated and controlled, and the cooling medium can be used as a crystal nucleus to promote crystallization, so that supercooling is avoided; the synergistic effect of the two can ensure that the gas product can be efficiently cooled, and simultaneously effectively prevent the equipment from being blocked in the cooling process.
The present invention is described in detail by the above embodiments, but the present invention is not limited to the above detailed structural features, which means that the present invention must not be implemented by the above detailed structural features. It should be understood by those skilled in the art that any modifications, equivalent substitutions of selected elements of the present invention, additions of auxiliary elements, selection of specific forms, etc., are intended to fall within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.

Claims (10)

1. The anti-blocking cooling crystallizer is characterized by comprising a shell (1), wherein the upper part of the shell (1) is provided with an air inlet (2), an air outlet (3), a cooling medium nozzle (4) and a protective gas inlet (5), and the bottom of the shell (1) is provided with a discharge hole (6);
a cooling wall interlayer (7) is arranged in the shell (1), the cooling wall interlayer (7) is a semi-sealed structure with a cavity (71), and the cavity (71) is opened at one side of the cooling wall interlayer (7) and is connected to the protective gas inlet (5); the stave interlayer (7) comprises a first stave (72) facing the air inlet (2) and a second stave (74) opposite to the first stave (72) and facing away from the air inlet (2); the first cooling wall (72) is provided with fine holes (73) which are arranged in an array mode, and the protective gas in the cavity (71) forms a gas wall facing the gas inlet (2) in the shell (1).
2. Anti-clogging cooling crystallizer according to claim 1, characterized in that said air inlet (2) is provided on the side wall of said shell (1), said cooling medium nozzle (4) being provided on the top surface of said shell (1) and between said air inlet (2) and said first cooling wall (72);
preferably, the air outlet (3) is provided on a side wall of the other side of the housing (1) opposite to the air inlet (2).
3. The crystallizer according to claim 2, characterized in that the inlet (5) for shielding gas is arranged on the top surface of the shell (1) between the nozzle (4) for cooling medium and the outlet (3);
preferably, the horizontal distance between the shielding gas inlet (5) and the side wall where the gas inlet (2) is located accounts for 30% -70% of the horizontal distance between the side wall where the gas inlet (2) is located and the side wall where the gas outlet (3) is located.
4. Anti-clogging cooling crystallizer according to any one of claims 1 to 3, characterized in that said array of fine holes (73) on said first cooling wall (72) is in a honeycomb arrangement;
preferably, the pore diameter of the fine pores (73) arranged in the array is 0.05-1 mm;
preferably, the total pore area of the fine pores (73) arranged in the array accounts for 70-95% of the surface area of one side of the first cooling wall (72);
preferably, from the inner surface of the first cooling wall (72) close to the cavity (71) to the outer surface far away from the cavity (71), each of the arrayed fine holes (73) is inclined towards the bottom of the shell (1), and the horizontal included angle of the arrayed fine holes (73) is 0-20 degrees.
5. Anti-clogging cooling crystallizer as claimed in any one of claims 1 to 4, characterized in that said discharge port (6) is connected to relative air blowers (9);
preferably, in the shell (1), the side wall where the air outlet (3) is located is provided with a slope (8) which extends towards the discharge hole in an inclined manner.
6. The crystallizer according to any one of claims 1 to 5, characterized in that the material of said shell (1) and the material of said cooling wall interlayer (7) comprise a first material and a second material;
preferably, the first material comprises carbon steel and/or glass fiber reinforced plastics;
preferably, the second material comprises any one of stainless steel, pure titanium, polytetrafluoroethylene or pure nickel or a combination of at least two of the stainless steel, the pure titanium, the polytetrafluoroethylene or the pure nickel;
preferably, the outer wall of the shell (1) is made of a first material, and the inner wall of the shell (1) is made of a second material;
preferably, the outer wall of the cooling wall interlayer (7) is made of a second material, and the inner wall of the cooling wall interlayer (7) is made of a first material;
preferably, heating wires and/or heat-insulating layers are mounted on the outside of the housing (1).
7. Anti-clogging cooling crystallizer according to any one of claims 1 to 6, characterized in that the cooling medium nozzles (4) comprise any one of round, spiral, hollow coniform or pipe nozzle openings.
8. A cooling crystallization method, characterized in that the method employs the anti-clogging cooling crystallizer of any one of claims 1-7, and the method comprises the following steps:
s1, injecting a cooling medium into the shell (1) from the cooling medium nozzle (4); protective gas is fed into a cavity (71) of the cooling wall interlayer (7) through a protective gas inlet (5), and an air wall facing the air inlet (2) is formed by the fine holes (73) arranged in the array on the first cooling wall (72);
s2, conveying the product to be cooled into the shell (1) from the air inlet (2), contacting with a cooling medium for cooling, and discharging the obtained solid product from the discharge hole (6) after the obtained solid product falls to the bottom of the shell (1) for collection.
9. The cooling crystallization method as claimed in claim 8, characterized in that the velocity of the cooling medium passing through the cooling medium nozzle (4) is 1-60 cm/s;
preferably, the speed of the protective gas passing through the protective gas inlet (5) is 1-60 cm/s;
preferably, the speed of the product to be cooled through the air inlet (2) is 1-20 cm/s.
10. Use of a cooling crystallization process according to claim 8 or 9 in the treatment of fly ash by chlorination.
CN202211425239.4A 2022-11-14 2022-11-14 Anti-blocking cooling crystallizer, cooling crystallization method and application thereof Pending CN115738348A (en)

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CN113786640A (en) * 2021-11-01 2021-12-14 内蒙古久泰新材料有限公司 Cyclic lactide production device and production method
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JPH0240203A (en) * 1988-07-29 1990-02-09 Nippon Steel Chem Co Ltd Method and device for collecting sublimated organic compound
US20020053288A1 (en) * 2000-11-08 2002-05-09 Tsukasa Takahashi Method for collecting reversely subliming substance and apparatus therefor
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