CN113893795B - Continuous aging device and method in pseudo-boehmite preparation process - Google Patents
Continuous aging device and method in pseudo-boehmite preparation process Download PDFInfo
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Abstract
The invention discloses a device and a method for uniformly and rapidly heating and continuously aging feed liquid in a pseudo-boehmite preparation process. The specific method comprises the following steps: the pseudo-boehmite feed liquid obtained through chemical synthesis enters a rapid heating continuous aging device, and firstly, the pseudo-boehmite feed liquid is directly contacted with steam with a certain temperature in a rapid heating area to realize uniform and rapid heating; and then directly entering a continuous aging zone, wherein the pseudo-boehmite feed liquid and the heating medium indirectly exchange heat so as to keep the feed liquid at a constant temperature, and realizing continuous aging treatment. The invention realizes the uniform and rapid temperature-rising continuous aging treatment of the feed liquid, can be matched with the continuous preparation process of pseudo-boehmite, and greatly improves the production efficiency and quality of the pseudo-boehmite.
Description
Technical Field
The invention belongs to the field of liquid heat treatment, and particularly relates to a device and a method for realizing uniform and rapid temperature rise and continuous aging of feed liquid in a pseudo-boehmite preparation process by using a supergravity technology.
Background
The aging treatment is also called hydrothermal treatment, aging, heat treatment, aging, etc., and is a method of heating a liquid phase and maintaining a certain temperature and treating a certain substance in the liquid phase. In the preparation process of inorganic metal hydroxides such as aluminum hydroxide, magnesium hydroxide, cerium hydroxide and zirconium hydroxide, the metal hydroxide feed liquid is prepared by chemical synthesis, the metal hydroxide has extremely small granularity, and the crystal form has poor stability and lower crystallinity, so that the metal hydroxide feed liquid needs to be subjected to aging treatment, the crystal grows, the crystallinity is improved, and the crystal form is uniform and stable. The aging treatment temperature is generally 30-100 ℃, and the constant temperature time is 0.5-3 h.
Pseudo-boehmite, also called pseudo/quasi/pseudo-boehmite, gelatinous boehmite and boehmite-like boehmite, is a transition product with uncertain composition, incomplete crystallization from disordered to ordered, weak crystalline state to crystalline state, and has a similar crystal structure as boehmite, but small crystals and poor crystallinity; the product is also a nontoxic, odorless white gelatinous (wet product) or powdery (dry product) product, has the characteristics of small granularity, high pore volume, large specific surface area, good peptization performance, high crystalline phase purity and thixotropy, is extremely easy to dissolve in strong acid and strong alkali, and has the moisture absorption phenomenon when the dry powder is exposed in the air. Pseudo-boehmite is mainly used as a binder of catalysts and an aluminum source for synthesizing molecular sieves, and is also commonly used for catalysts and catalyst carriers.
The main preparation methods of pseudo-boehmite include a carbonization method, an acid method, an alkali method, an aluminum alcohol method, a sol-gel method, a seed precipitation method and the like. In the preparation process of different methods, the pseudo-boehmite feed liquid needs to be aged, the crystallinity and stability of the pseudo-boehmite are improved, the aging temperature is generally 50-95 ℃, and the constant temperature time is 0.5-2 h. In industrial practice, the equipment used for the ageing treatment is a bubble-tank type equipment. And (3) introducing water vapor into the kettle, directly contacting with the feed liquid, heating the feed liquid, stopping introducing the water vapor after the feed liquid reaches the aging temperature, monitoring the temperature of the liquid material in real time, intermittently introducing the water vapor if the temperature is reduced, and compensating heat loss, thereby keeping the constant temperature in the kettle, and keeping the feed liquid in the kettle for a certain time to realize constant-temperature aging treatment of the feed liquid. The high-pressure high-temperature heat treatment is widely applied to a heating reaction kettle in laboratories and industrial production, and the heating reaction kettle is sealed and heated in a water, oil, gas and electric heating mode, so that a constant-pressure constant-temperature timing process is realized.
The bubbling kettle type equipment and the heating reaction kettle are both intermittent treatment modes, and the problems of uneven heating, overhigh local temperature rise, steam waste and the like exist. In industrial production, a large amount of hot steam is required to be introduced into the feed liquid by using bubbling kettle type equipment for aging treatment, and the problems of insufficient contact between the feed liquid and the steam, uneven heating and the like are caused due to the limitation of the bubbling kettle type equipment, so that the uniformity of crystal particle size and performance is poor, the quality of products is influenced, and the fine application of the products is severely restricted; meanwhile, the bubbling kettle type equipment has poor mass transfer and heat transfer capability, so that a great deal of steam is wasted. Meanwhile, the treatment method is an intermittent process, and the production time difference between the treatment method and the front and back working sections is large, so that the production capacity of the front and back working sections is not matched, and the production capacity and efficiency of the process are severely restricted.
Disclosure of Invention
The invention provides a device and a method for uniformly and rapidly heating and continuously aging feed liquid in a pseudo-boehmite preparation process, which can solve a plurality of problems existing in the prior equipment and process. The invention combines the supergravity technology with the pseudo-boehmite preparation process, and realizes the uniform and rapid heating continuous aging process of the feed liquid.
The invention provides a device for uniformly and rapidly heating and continuously aging feed liquid in a pseudo-boehmite preparation process, which is an integrated device for uniformly and rapidly heating and continuously aging feed liquid at constant temperature. The device is divided into a rapid heating area and a continuous ageing area, wherein the rapid heating area is provided with a supergravity vapor-liquid direct heat exchange device, and the continuous ageing area is provided with a tubular continuous ageing device. The liquid outlet of the supergravity steam-liquid direct heat exchange device of the rapid temperature rise region is the liquid inlet of the continuous ageing region tubular continuous ageing device, and the feed liquid directly enters the continuous ageing region after being treated by the rapid temperature rise region.
The invention relates to a supergravity vapor-liquid direct heat exchange device, which comprises a motor, a liquid inlet, a liquid distributor, a liquid outlet, a gas inlet, a gas outlet, a packing layer, a shell heat preservation layer and a shell. The motor is directly connected with the packing layer to drive the packing layer to rotate; the inside of the packing layer is provided with silk screen packing or pall ring packing; the bottom of the equipment is provided with a gas inlet and a liquid outlet, the top of the equipment is provided with a gas outlet and a liquid inlet, the liquid inlet is connected with a liquid distributor, the liquid distributor is inserted into the axis of the packing layer, and the liquid outlet of the equipment is a connection port connected with the continuous aging zone; the shell is provided with a shell heat-insulating layer outside.
And the continuous aging area is provided with tubular continuous aging equipment for continuous constant-temperature aging process of the feed liquid. The material liquid heated in the rapid heating area is conveyed to a heat preservation tube array to form W-shaped vertical direction and flow in multiple layers; a heating medium baffle plate is arranged in the area, and after the heating medium enters the equipment, the heating medium flows in M type and multiple layers in the vertical direction outside the heat insulation tube array; the heating medium and the feed liquid are subjected to indirect heat exchange between the pipes, the flowing time of the feed liquid is constant-temperature aging time, and constant-temperature continuous aging treatment of the feed liquid is realized.
The invention relates to a tubular continuous ageing device which comprises a liquid inlet, a liquid outlet, a heating medium inlet, a heating medium outlet, a heat preservation tube array, a heating medium baffle plate, a shell heat preservation layer and a shell. The liquid inlet and the liquid outlet are communicated with the heat-preserving tube array, and the liquid inlet is a connecting port which is directly connected with the rapid heating area; the heating medium baffle plates are arranged between the vertical layers and the vertical columns of the heat preservation column pipes; the shell outer layer is provided with a shell heat-insulating layer.
The heat-insulating tubes are arranged in a front-back multilayer manner in the vertical direction, and each layer of tubes are arranged in a W-shaped manner from left to right in the vertical direction. Therefore, the feed liquid in the heat insulation tube array is in a W shape from left to right in the vertical direction and flows in multiple layers from front to back in a progressive manner. The arrangement mode, the pipe diameter and the length of the tube array are designed, and the flow speed and the flow time of the feed liquid are controlled, so that the ageing time of the feed liquid is determined.
The heating medium baffle plate of the invention comprises a layer baffle plate and a vertical baffle plate. A vertical baffle plate is arranged in the vertical direction inside the shell of the tubular continuous ageing equipment, the top end or the bottom end of the vertical baffle plate is fixedly arranged with the inner wall of the shell, the plate height of the vertical baffle plate is smaller than the height of the shell, the plate length is the same as the width of the shell, and the vertical baffle plate is arranged between W-shaped tubes and penetrates front and back; when the vertical baffle plate is arranged at the lower bottom of the inner wall of the shell, a blank area is reserved between the vertical baffle plate and the top of the shell; when the vertical baffle plate is arranged on the upper top of the inner wall of the shell, a blank area is reserved between the vertical baffle plate and the lower bottom of the shell, and the vertical baffle plate is arranged in a staggered manner. The vertical baffle plate can guide the heating medium to flow in a vertical direction from left to right in an M shape, and the heating medium flows in the same direction or in the opposite direction with the feed liquid in the tube array to perform indirect heat exchange. The layer baffle plates are arranged between layers of the heat-insulating tubes which are arranged in a front-back multilayer manner in the vertical direction, and the layer baffle plates and the vertical baffle plates are vertically arranged in the shell and are mutually perpendicular and crossed. One side of the upper part of the layer baffle plate is provided with a through hole which is an inlet for the heating medium to enter the next layer of flow space, the position of the through hole is the same as that of the heat preservation tubulation entering the next layer, and connecting pipelines among the heat preservation tubulations of all layers penetrate through the through hole, so that the heating medium and the feed liquid flow from front to back in multiple layers simultaneously.
According to the method for uniformly and rapidly heating and continuously aging the feed liquid in the pseudo-boehmite preparation process, the pseudo-boehmite feed liquid obtained through chemical synthesis enters a rapid heating and continuously aging device, and firstly, the pseudo-boehmite feed liquid is directly contacted with steam with a certain temperature in a rapid heating area to realize uniform and rapid heating; and then directly entering a continuous aging zone, wherein the pseudo-boehmite feed liquid and the heating medium indirectly exchange heat so as to keep the feed liquid at a constant temperature, and realizing continuous aging treatment.
The pseudo-boehmite feed liquid is a liquid containing pseudo-boehmite and intermediate products thereof in the pseudo-boehmite preparation process.
The method for continuously aging the feed liquid by uniformly and rapidly heating comprises the following specific operation steps: switching on a power supply, driving the packing layer to rotate at a high speed by a motor, conveying feed liquid by a liquid pump, controlling the flow of the feed liquid through a vortex shedding flowmeter, introducing the feed liquid into a liquid inlet, and entering the packing layer through a liquid distributor; the saturated or overheated steam is controlled in flow rate through an electromagnetic flowmeter, and is introduced into a gas inlet to enter a rapid heating zone; in the super-gravity environment, the feed liquid flows from inside to outside along the radial direction of the filler, and the steam is directly contacted with the feed liquid for heating; the heated feed liquid directly enters a heat preservation tube array of the continuous aging zone, a heating medium is introduced into a heating medium inlet through an electromagnetic flowmeter, flows outside the heat preservation tube array under the action of a heating medium baffle plate, and carries out indirect heat exchange between the heating medium and the feed liquid; the feed liquid continuously flows in the heat-insulating tube array and flows out from the liquid outlet, thus completing continuous constant-temperature aging treatment.
The aging treatment conditions of the invention are as follows: the aging temperature is 30-100 ℃, the rotating speed is 100-3000 rpm, and the aging time is 0.1-3 h; the heating medium of the continuous aging treatment zone is hot air or flue gas, and the temperature is 30-120 ℃ in a normal pressure state.
The innovation point of the invention is that: (1) the supergravity technology is a chemical process strengthening means for strengthening gas-liquid, liquid-liquid mass transfer and reaction by utilizing a rotating packed bed, and is applied to unit operations such as separation, reaction, crystallization, rectification and the like, so that the technology is widely applied to the industries such as chemical industry, environmental protection, military industry and the like. (2) The invention carries out the uniform and rapid heating treatment of the feed liquid in the rapid heating zone, and can realize the uniform and rapid heating of the pseudo-boehmite feed liquid: by utilizing the supergravity vapor-liquid direct heat exchange equipment, the liquid distributor is used for uniformly distributing and rotating the filler at a high speed, the liquid is highly dispersed by the filler to become liquid drops, liquid wires and liquid films which are directly contacted with steam, so that the contact area of the liquid and the steam is greatly increased, the heat exchange efficiency is improved, the mass transfer and the heat transfer are simultaneously carried out, the vapor-liquid mass transfer and heat transfer process is rapidly completed, the liquid reaches the aging temperature, the problems of local overheating in the liquid heating process and product quality reduction are effectively avoided, and the uniform and rapid heating of the liquid is realized; meanwhile, the steam utilization rate is high, and the steam waste phenomenon is improved. (3) In the rapid heating zone, steam is used as a heating medium: the steam and the feed liquid are in direct contact with each other in the temperature rising process, the steam transfers mass to the feed liquid, the concentration of the feed liquid is reduced, the growth of crystals is not influenced, and the production cost of the steam is low compared with that of hot air. If hot air is used for heat transfer, the feed liquid transfers mass to the gas phase, and the water in the liquid phase generates steam, so that the concentration of the feed liquid is increased, the viscosity of the feed liquid is increased, equipment is easily blocked, and adverse effects are caused.
The invention has the beneficial effects that:
the invention relates to a method and a device for continuously aging feed liquid in a uniform and rapid heating manner in the preparation process of pseudo-boehmite, which are suitable for the aging process of different pseudo-boehmite preparation methods, such as a carbon separation method, an acid method, an alkali method, an aluminum alcohol method, a sol-gel method, a seed separation method and the like. Meanwhile, the method is also suitable for aging treatment in the preparation process of aluminum hydroxide with different crystal forms and other inorganic metal hydroxides. The invention can realize the uniform and rapid temperature-rising continuous aging treatment of the feed liquid, can be matched with the continuous preparation process of pseudo-boehmite, and greatly improves the production efficiency and quality of the pseudo-boehmite.
Drawings
FIG. 1 shows a rapid thermal aging apparatus according to the present invention.
Fig. 2 is a three-view of the structure of the continuous aging zone in the rapid heating continuous aging device of the present invention.
Fig. 3 is a schematic diagram of a flow direction of a heating medium in a continuous aging zone in a method for uniformly and rapidly heating and continuously aging a feed liquid in a pseudo-boehmite preparation process according to the present invention.
FIG. 4 is a schematic view of a heating medium baffle plate in the rapid heating continuous aging device of the invention.
In the figure: 1: a rapid heating zone; 2: a continuous aging zone; 3: a liquid inlet; 4: a liquid distributor; 5: a filler layer; 6: a connection port; 7: a gas inlet; 8: a gas outlet; 9: heat preservation tube array; 10: a liquid outlet; 11: a heating medium inlet; 12: a heating medium baffle; 13: a heating medium outlet; 14: a shell insulation layer; 12.1: a vertical baffle; 12.2: a layer baffle; 12.2.1: layer baffle through holes. A is steam, B is feed liquid, and C is heating medium. FD is flowing from top to bottom and FU is flowing from bottom to top.
Detailed Description
The present invention is further illustrated by, but not limited to, the following examples.
As shown in figures 1-4, the invention provides a device for uniformly and rapidly heating and continuously aging feed liquid in the preparation process of pseudo-boehmite, which is an integrated device for uniformly and rapidly heating treatment process and constant-temperature continuous aging treatment process of aggregate liquid. The device is divided into a rapid heating zone 1 and a continuous ageing zone 2, wherein the rapid heating zone 1 is provided with a supergravity vapor-liquid direct heat exchange device, and the continuous ageing zone 2 is provided with a tubular continuous ageing device. The liquid outlet of the high gravity gas-liquid direct heat exchange device of the rapid temperature rise region 1 is the liquid inlet of the continuous ageing region 2 tubular continuous ageing device, and is a connection port 6, and the feed liquid directly enters the continuous ageing region 2 after being processed by the rapid temperature rise region 1.
The invention relates to a supergravity vapor-liquid direct heat exchange device, which comprises a motor, a liquid inlet 3, a liquid distributor 4, a liquid outlet (a connecting port 6), a gas inlet 7, a gas outlet 8, a packing layer 5, a shell heat preservation layer 14 and a shell. The motor is directly connected with the packing layer 5 to drive the packing layer to rotate; the inside of the packing layer is provided with silk screen packing or pall ring packing; the bottom of the equipment is provided with a gas inlet 7 and a liquid outlet, the top of the equipment is provided with a gas outlet 8 and a liquid inlet 3, the liquid inlet 3 of the equipment is connected with a liquid distributor 4, the liquid distributor 4 is inserted into the axis of a packing layer 5, and the liquid outlet of the equipment is a connecting port 6 connected with a continuous aging zone; the shell is provided with a shell heat-insulating layer 14 outside.
And the continuous aging area is provided with tubular continuous aging equipment for continuous constant-temperature aging process of the feed liquid. The material liquid heated in the rapid heating area 1 is conveyed to a heat preservation tube array 9 to form W-shaped vertical direction and flow in multiple layers in a progressive manner; a heating medium baffle plate 12 is arranged in the area, and after the heating medium enters the equipment, the heating medium flows in a vertical M-shaped direction and in multiple layers outside the heat insulation tube array 9; the heating medium and the feed liquid are subjected to indirect heat exchange between the pipes, the flowing time of the feed liquid is constant-temperature aging time, and constant-temperature continuous aging treatment of the feed liquid is realized.
The invention relates to a tubular continuous ageing device which comprises a liquid inlet (a connecting port 6), a liquid outlet 10, a heating medium inlet 11, a heating medium outlet 13, a heat insulation tube array 9, a heating medium baffle plate 12, a shell heat insulation layer 14 and a shell. The liquid inlet and the liquid outlet are communicated with the heat-preserving tube array 9, and the liquid inlet is a connecting port 6 which is directly connected with the rapid heating area; the heating medium baffle plates 12 are arranged between the vertical layers and the vertical columns of the heat insulation tube array 9; the shell outer layer is provided with a shell heat preservation layer 14.
The heat-insulating tubes 9 are arranged in a vertical direction in a front-back multi-layer manner, and each layer of tubes is arranged in a W-shaped manner from left to right in the vertical direction. Thus, the liquid material flows in the heat-insulating tube array 9 in a vertical direction from left to right in a W-shaped manner and in a multi-layer progressive manner from front to back. The arrangement mode, the pipe diameter and the length of the tube array are designed, and the flow speed and the flow time of the feed liquid are controlled, so that the ageing time of the feed liquid is determined.
The heating medium baffle plate of the invention comprises two vertical baffle plates 12.1 and a layer baffle plate 12.2. A vertical baffle plate 12.1 is arranged in the vertical direction inside the shell of the tubular continuous ageing equipment, the top end or the bottom end of the vertical baffle plate 12.1 is fixedly arranged with the inner wall of the shell, the plate height of the vertical baffle plate is smaller than the height of the shell, the plate length is the same as the width of the shell, and the vertical baffle plate 12.1 is arranged between the W-shaped heat-preserving pipes 9 and penetrates front and back; when the vertical baffle plate 12.1 is arranged at the lower bottom of the inner wall of the shell, a blank area is reserved between the vertical baffle plate and the top of the shell; when the vertical baffle plate is arranged on the upper top of the inner wall of the shell, a blank area is reserved between the vertical baffle plate and the lower bottom of the shell, and the vertical baffle plate is arranged in a staggered manner. The vertical baffle plates 12.1 can guide the heating medium to flow from left to right in a vertical direction in an M shape, and the heating medium flows in the same direction or in the opposite direction with the feed liquid in the tube array to perform indirect heat exchange. The layer baffle plates 12.2 are arranged between layers of heat-insulating tubes which are arranged in a plurality of layers in the front-back direction in the vertical direction, and the layer baffle plates 12.2 and the vertical baffle plates 12.1 are vertically arranged in the shell and vertically crossed with each other. One side (upper left end or upper right end) of the upper part of the layer baffle plate 12.2 is provided with a layer baffle plate through hole 12.2.1, namely an inlet for a heating medium to enter a next layer of laminar flow space, the position of the layer baffle plate through hole 12.2.1 and the position of the heat preservation tubulation 9 to enter the next layer are the same, and connecting pipelines among the heat preservation tubulation of all layers penetrate through the through holes, so that the heating medium and the feed liquid simultaneously flow from front to back in multiple layers.
According to the method for uniformly and rapidly heating and continuously aging the feed liquid in the pseudo-boehmite preparation process, the pseudo-boehmite feed liquid obtained through chemical synthesis enters a rapid heating and continuously aging device, and firstly, in a rapid heating area, the pseudo-boehmite feed liquid B is directly contacted with saturated or overheated steam A to realize uniform and rapid heating; then directly enters a continuous aging zone, and the pseudo-boehmite feed liquid B and the heating medium C exchange heat indirectly to keep the feed liquid B at a constant temperature, so that continuous aging treatment is realized.
The pseudo-boehmite feed liquid B is a liquid containing pseudo-boehmite and intermediate products thereof in the pseudo-boehmite preparation process.
The method for continuously aging the feed liquid by uniformly and rapidly heating comprises the following specific operation steps: switching on a power supply, driving the packing layer to rotate at a high speed by a motor, conveying feed liquid by a liquid pump, controlling the flow of the feed liquid through a vortex shedding flowmeter, introducing the feed liquid into a liquid inlet, and entering the packing layer through a liquid distributor; the saturated or overheated steam is controlled in flow rate through an electromagnetic flowmeter, and is introduced into a gas inlet to enter a rapid heating zone; in the super-gravity environment, the feed liquid flows from inside to outside along the radial direction of the filler, and the steam is directly contacted with the feed liquid for heating; the heated feed liquid directly enters a heat preservation tube array of the continuous aging zone, a heating medium is introduced into a heating medium inlet through an electromagnetic flowmeter, flows outside the heat preservation tube array under the action of a heating medium baffle plate, and carries out indirect heat exchange between the heating medium and the feed liquid; the feed liquid continuously flows in the heat-insulating tube array and flows out from the liquid outlet, thus completing continuous constant-temperature aging treatment.
The aging treatment conditions of the invention are as follows: the aging temperature is 30-100 ℃, the rotating speed is 100-3000 rpm, and the aging time is 0.1-3 h; the heating medium of the continuous aging treatment zone is hot air or flue gas, and the temperature is 30-120 ℃ in a normal pressure state.
The following describes a specific implementation of the above scheme by means of specific examples.
Example 1: in the process for preparing pseudo-boehmite by a carbonization method, pseudo-boehmite slurry is obtained after carbonization reaction, the state is normal temperature and pressure, and the heat treatment condition is 90 ℃ and the temperature is kept for 1h. The flow rate of the slurry is 100L/h, the flow rate of steam required for reaching 90 ℃ is 15L/h, the feed liquid enters a pipeline and flows for 1h, the pipe diameter of a heat exchange tube array is 65mm, and the length of the heat exchange tube array is 30m.
Example 2: in the process for preparing aluminum hydroxide by a carbonization method, aluminum hydroxide slurry is obtained after carbonization reaction, the state is normal temperature and normal pressure, the aging temperature is 70 ℃, and the aging time is 0.5h. The flow rate of the slurry is 100L/h, the flow rate of the steam required for reaching 70 ℃ is 9.5L/h, the feed liquid enters the pipeline and flows for 0.5h, the pipe diameter of the heat exchange tube array is 50mm, and the length of the heat exchange tube array is 25m.
Example 3: in the process of preparing magnesium hydroxide by a liquid phase precipitation method, magnesium hydroxide slurry is obtained after reaction, the state is normal temperature and normal pressure, the heat treatment condition is 50 ℃, and the temperature is kept for 0.25h. The flow rate of the slurry is 100L/h, the flow rate of the steam required for reaching 50 ℃ is 5.5L/h, the feed liquid enters the pipeline and flows for 0.25h, the pipe diameter of the heat exchange tube array is 40mm, and the length of the heat exchange tube array is 20mm.
Example 4: in the liquid phase precipitation method for preparing cerium hydroxide, cerium hydroxide slurry is obtained after reaction, the state is normal temperature and normal pressure, and the heat treatment condition is 50 ℃ and the temperature is kept for 0.5h. The flow rate of the slurry is 100L/h, the flow rate of the steam required for reaching 50 ℃ is 5.5L/h, the feed liquid enters the pipeline and flows for 0.5h, the pipe diameter of the heat exchange tube array is 50mm, and the length of the heat exchange tube array is 25m.
Claims (8)
1. The utility model provides a continuous ageing device of feed liquid even quick intensification in pseudo-boehmite preparation process which characterized in that: the device is divided into a rapid heating zone and a continuous aging zone, wherein the rapid heating zone is provided with a supergravity vapor-liquid direct heat exchange device, and the continuous aging zone is provided with a tubular continuous aging device; the liquid outlet of the supergravity steam-liquid direct heat exchange device of the rapid temperature rise region is the liquid inlet of the tubular continuous aging device of the continuous aging region, and the feed liquid directly enters the continuous aging region after being treated by the rapid temperature rise region;
the tubular continuous ageing equipment is used for carrying out continuous constant-temperature ageing process of the feed liquid; the device comprises a liquid inlet, a liquid outlet, a heating medium inlet, a heating medium outlet, a heat preservation tube array, a heating medium baffle plate, a shell heat preservation layer and a shell; the liquid inlet is communicated with the heat-preserving tube array, and is a connecting port directly connected with the rapid heating area; the heating medium baffle plates are arranged between the vertical layers and the vertical columns of the heat preservation column pipes; the outer layer of the shell is provided with a shell heat-insulating layer;
the heat-insulating tubes are arranged in a front-back multilayer manner in the vertical direction, and each layer of heat-insulating tubes are arranged in a W-shaped manner from left to right in the vertical direction; the feed liquid is in a W shape in the vertical direction in the heat insulation tube array and flows progressively from front to back in multiple layers;
the heating medium baffle plate comprises a layer baffle plate and a vertical baffle plate, wherein the vertical baffle plate is arranged in the vertical direction in the shell of the tubular continuous ageing equipment, the top end or the bottom end of the vertical baffle plate is fixedly arranged with the inner wall of the shell, the layer baffle plate is arranged between layers of heat-insulating tubes which are arranged in a front-back multilayer manner in the vertical direction, and the layer baffle plate and the vertical baffle plate are vertically arranged in the shell and are mutually vertically crossed; a through hole is formed in one side of the upper part of the layer baffle plate, namely an inlet for a heating medium to enter a next layer of flow space, the through hole is the same as the position of the heat preservation tube array entering the next layer, and connecting pipelines among the heat preservation tube arrays of all layers penetrate through the through hole, so that the heating medium and the feed liquid flow from front to back in multiple layers simultaneously;
the plate height of the vertical baffle plate is smaller than the height of the shell, the plate length is the same as the width of the shell, and the vertical baffle plate is arranged between the W-shaped tubes and penetrates front and back; when the vertical baffle plate is arranged at the lower bottom of the inner wall of the shell, a blank area is reserved between the vertical baffle plate and the top of the shell; when the vertical baffle plate is arranged on the upper top of the inner wall of the shell, a blank area is reserved between the vertical baffle plate and the lower bottom of the shell, and the vertical baffle plate is arranged in a staggered manner up and down; the vertical baffle plate guides the heating medium to flow in the vertical direction in an M shape, and the heating medium flows in the same direction or in the opposite direction with the feed liquid in the tube array to perform indirect heat exchange.
2. The device for uniformly and rapidly heating and continuously aging feed liquid in pseudo-boehmite preparation process according to claim 1, wherein the device comprises the following components: the super-gravity vapor-liquid direct heat exchange device comprises a motor, a liquid inlet, a liquid distributor, a liquid outlet, a gas inlet, a gas outlet, a packing layer, a shell heat preservation layer and a shell, wherein the motor is directly connected with the packing layer to drive the packing layer to rotate; the inside of the packing layer is provided with silk screen packing or pall ring packing; the bottom of the equipment is provided with a gas inlet and a liquid outlet, the top of the equipment is provided with a gas outlet and a liquid inlet, the liquid inlet is connected with a liquid distributor, the liquid distributor is inserted into the axis of the packing layer, and the liquid outlet of the equipment is a connection port connected with the continuous aging zone; the shell is provided with a shell heat-insulating layer outside.
3. A method for uniformly and rapidly heating and continuously aging feed liquid in the process of preparing pseudo-boehmite, which adopts the device for uniformly and rapidly heating and continuously aging feed liquid in the process of preparing pseudo-boehmite according to any one of claims 1-2, and is characterized in that: the pseudo-boehmite feed liquid obtained through chemical synthesis enters a rapid heating continuous aging device, and firstly, the pseudo-boehmite feed liquid is in direct contact with steam in a rapid heating area to realize uniform and rapid heating; and then directly enters a continuous aging zone, wherein the pseudo-boehmite feed liquid and a heating medium indirectly exchange heat so that the feed liquid keeps constant temperature, and continuous aging treatment is realized.
4. The method for uniformly and rapidly heating and continuously aging the feed liquid in the preparation process of pseudo-boehmite according to claim 3, which is characterized in that: the pseudo-boehmite feed liquid is a liquid containing pseudo-boehmite and intermediate products thereof in the pseudo-boehmite preparation process.
5. The method for uniformly and rapidly heating and continuously aging the feed liquid in the preparation process of pseudo-boehmite according to claim 3, which is characterized in that: the operation steps are as follows: switching on a power supply, driving the packing layer to rotate at a high speed by a motor, conveying feed liquid by a liquid pump, controlling the flow of the feed liquid through a vortex shedding flowmeter, introducing the feed liquid into a liquid inlet, and entering the packing layer through a liquid distributor; the saturated or overheated steam is controlled in flow rate by a vortex shedding flowmeter, and is introduced into a gas inlet to enter a rapid heating zone; in the super-gravity environment, the feed liquid flows from inside to outside along the radial direction of the filler, and the steam is directly contacted with the feed liquid for heating; the heated feed liquid directly enters a heat preservation tube array of the continuous aging zone, a heating medium is introduced into a heating medium inlet through an electromagnetic flowmeter, flows outside the heat preservation tube array under the action of a heating medium baffle plate, and carries out indirect heat exchange between the heating medium and the feed liquid; the feed liquid continuously flows in the heat-insulating tube array and flows out from the liquid outlet, thus completing continuous constant-temperature aging treatment.
6. The method for uniformly and rapidly heating and continuously aging the feed liquid in the preparation process of pseudo-boehmite according to claim 5, which is characterized in that: aging treatment conditions: the aging temperature is 30-100 ℃, the rotating speed is 100-3000 rpm, and the aging time is 0.1-3 h.
7. The method for uniformly and rapidly heating and continuously aging the feed liquid in the preparation process of pseudo-boehmite according to claim 5, which is characterized in that: the heating medium of the continuous aging treatment zone is hot air or flue gas, and the temperature is 30-120 ℃ in a normal pressure state.
8. The method for uniformly and rapidly heating and continuously aging the feed liquid in the preparation process of pseudo-boehmite according to claim 3, which is characterized in that: the pseudo-boehmite can be replaced with an inorganic metal hydroxide including one of aluminum hydroxide, magnesium hydroxide, and cerium hydroxide.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1320802A (en) * | 2001-03-24 | 2001-11-07 | 华南理工大学 | Axial flow-type heat exchanger with convergent-divergent tube, full counterflow and dual shell passes and its heat-exchange method |
| CN101078597A (en) * | 2006-05-22 | 2007-11-28 | 北京美联桥科技发展有限公司 | U-shape tube type heat exchanger |
| CN203550683U (en) * | 2013-09-24 | 2014-04-16 | 贵阳铝镁设计研究院有限公司 | Heat exchanger for pre-desilicication heating |
| CN210449192U (en) * | 2019-08-16 | 2020-05-05 | 南京禧通祥盛科技发展有限公司 | Preparation device of active superfine aluminum hydroxide |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348490C (en) * | 2005-01-06 | 2007-11-14 | 北京化工大学 | Ultra-fine whisker type modified aluminum hydroxide and its preparation method |
| CN100419366C (en) * | 2005-07-27 | 2008-09-17 | 西安华广电站锅炉有限公司 | High efficiency plate pipe reverse running type square box heat exchanger |
| US9289739B2 (en) * | 2009-06-23 | 2016-03-22 | Chevron Philips Chemical Company Lp | Continuous preparation of calcined chemically-treated solid oxides |
| CN104174343B (en) * | 2013-05-22 | 2018-02-16 | 中石化洛阳工程有限公司 | A kind of liquid acid alkylation reactor |
| CN105600812B (en) * | 2015-12-24 | 2017-05-10 | 江苏晶晶新材料有限公司 | Method for preparing high-viscosity and superfine pseudo boehmite coating adhesive |
| CN208829283U (en) * | 2018-07-18 | 2019-05-07 | 中国石油天然气股份有限公司 | Pseudo-boehmite synthesis aging device and pseudo-boehmite synthesis aging system |
| CN109395691A (en) * | 2018-12-22 | 2019-03-01 | 山东大明精细化工有限公司 | It is a kind of for producing the pipeline reactor and its application method of surfactant |
| CN211190193U (en) * | 2019-11-14 | 2020-08-07 | 淄博金力王工贸有限公司 | Aging device for pseudo-boehmite production |
| CN213376649U (en) * | 2020-08-20 | 2021-06-08 | 武汉有机实业有限公司 | Continuous reaction device for preparing benzyl acetate |
| CN112337130B (en) * | 2020-10-22 | 2022-04-22 | 中北大学 | Device and method for supergravity direct crystallization |
-
2021
- 2021-10-14 CN CN202111197447.9A patent/CN113893795B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1320802A (en) * | 2001-03-24 | 2001-11-07 | 华南理工大学 | Axial flow-type heat exchanger with convergent-divergent tube, full counterflow and dual shell passes and its heat-exchange method |
| CN101078597A (en) * | 2006-05-22 | 2007-11-28 | 北京美联桥科技发展有限公司 | U-shape tube type heat exchanger |
| CN203550683U (en) * | 2013-09-24 | 2014-04-16 | 贵阳铝镁设计研究院有限公司 | Heat exchanger for pre-desilicication heating |
| CN210449192U (en) * | 2019-08-16 | 2020-05-05 | 南京禧通祥盛科技发展有限公司 | Preparation device of active superfine aluminum hydroxide |
Non-Patent Citations (1)
| Title |
|---|
| 俸志荣 ; 焦纬洲 ; 余丽胜 ; 李晓霞 ; 王永红 ; 刘有智 ; .超重力过程工程装置结构研究进展.过程工程学报.2016,(03),全文. * |
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