CN112934118A - Calcium nitrate reaction device - Google Patents
Calcium nitrate reaction device Download PDFInfo
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- CN112934118A CN112934118A CN202110068712.7A CN202110068712A CN112934118A CN 112934118 A CN112934118 A CN 112934118A CN 202110068712 A CN202110068712 A CN 202110068712A CN 112934118 A CN112934118 A CN 112934118A
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- calcium nitrate
- tank
- reaction tank
- reaction
- nitric acid
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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
- B01J4/005—Feed or outlet devices as such, e.g. feeding tubes provided with baffles
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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
Abstract
The invention belongs to the technical field of inorganic compound fertilizer production and provides a calcium nitrate reaction device. The device includes the retort, and retort upper portion is close to tank deck department and is provided with the baffle, and the baffle centers on forming the collecting tank with the outer wall of retort, and on the jar wall of retort, a plurality of overflow mouths are seted up to the bottom that is close to the collecting tank, and the overflow mouth distributes around the circumference at retort jar wall place, and the overflow mouth is rectangular form, and the cambered surface distance between two adjacent overflow mouths is not more than 15. Owing to set up long banding overflow mouth, on the one hand, impurity such as the building stones of large granule is held back in the retort, realizes continuous production, and on the other hand, the impurity of small granule is difficult to deposit in overflow mouth department, effectively avoids the discharge gate to be blockked up. More importantly, the calcium nitrate solution is discharged from the periphery of the upper part of the reaction tank, so that the calcium nitrate solution is prevented from being discharged from a single outlet to cause the easy formation of an inherent liquid channel.
Description
Technical Field
The invention belongs to the technical field of inorganic compound fertilizer production, and particularly relates to a calcium nitrate reaction device.
Background
The calcium nitrate solution is usually generated by solid-liquid contact reaction of stone and nitric acid, and is one of indispensable raw materials for producing calcium ammonium nitrate fertilizer.
The stone and nitric acid contact reaction is generally carried out in a reaction vessel, for example, the Chinese patent with patent number 201621154398.5 provides a solid-liquid mixed material continuous reactor applied to calcium nitrate production, which comprises a reaction bin, an annular liquid outlet bin is fixed on the outer wall of the reaction bin, the annular liquid outlet bin is communicated with the reaction bin through a flange port, the flange port is arranged at the lower part of the annular liquid outlet bin, and a reaction liquid outlet is arranged at the upper part of the annular liquid outlet bin. The flange opening is obliquely fixed with a baffle, and the baffle and the flange opening form a clamping opening. Although the solid-liquid mixed material continuous reactor can realize the continuous contact reaction of the stone and the nitric acid, the following problems are present:
firstly, calcium nitrate solution generated after stone and nitric acid react contains easily-settled solid slag which is continuously deposited at a flange opening, so that the flange opening is easily blocked, normal discharging is influenced, and material overflow is caused;
secondly, the calcium nitrate solution is discharged from the flange opening, a fixed liquid channel is easily formed, namely, the nitric acid and the calcium nitrate solution flow out from the flange opening along the fixed channel, so that the contact area of the nitric acid and stone is reduced, the reaction rate is reduced, the content of the nitric acid in the discharging is increased, and the nitric acid is wasted.
Disclosure of Invention
In view of this, the invention provides a calcium nitrate reaction device, which solves the technical problems in the prior art that a discharge port is easy to block and a fixed liquid channel is easy to form in the production process of a calcium nitrate solution, so that the reaction rate is influenced.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a calcium nitrate reaction device comprises a reaction tank, wherein a baffle is arranged at the upper part of the reaction tank close to the tank top, a liquid collecting tank is formed by the baffle and the outer wall of the reaction tank in a surrounding manner, and a calcium nitrate discharging pipe fitting is arranged at the bottom of the liquid collecting tank; a plurality of overflow ports are formed in the tank wall of the reaction tank and close to the bottom of the liquid collecting tank, the overflow ports are distributed around the circumference of the tank wall of the reaction tank, and the overflow ports are long-strip-shaped and have the height larger than the width; the arc surface distance between two adjacent overflow ports is not more than 15 degrees, and the width of each overflow port is 0.5 cm-1.0 cm.
Preferably, the arc-shaped distance between two adjacent overflow ports is 5-10 degrees.
Preferably, the top of the reaction tank is provided with a stone feeding pipe fitting and a gas phase discharging pipe fitting, and the bottom of the reaction tank is provided with a nitric acid feeding distributor.
Preferably, the nitric acid feeding distributor is cross-shaped, and a plurality of nitric acid distributing holes are formed below the nitric acid feeding distributor.
Preferably, the reaction tank is further provided with a solid-liquid boundary position detection assembly, the solid-liquid boundary position detection assembly comprises a heavy hammer, a winch, a steering pulley block and a traction rope, the heavy hammer is arranged in the reaction tank, the winch is installed on the outer wall of the reaction tank, the steering pulley block is fixed on the tank top of the reaction tank, one end of the traction rope is connected with the heavy hammer, the other end of the traction rope penetrates through the tank top of the reaction tank, is erected on the steering pulley block and is wound on the winch; the winch rotates, and the traction rope can be wound on or released from the winch so as to lift the heavy hammer in the vertical direction.
Preferably, be provided with the calibrated scale on the outer wall of retort, the haulage rope is close to the one end of capstan winch is provided with the pointer, the orthographic projection of pointer can with the calibrated scale coincidence.
Preferably, the steering pulley block comprises at least one fixed pulley and a pulley mounting seat which are arranged side by side, the pulley mounting seat is fixed on the tank top of the reaction tank, and the fixed pulley is arranged in the pulley mounting seat.
Preferably, the area of the lower surface of the weight is not less than 50cm2。
Preferably, a locking member is provided on the winch.
According to the technical scheme, the invention provides a calcium nitrate reaction device, which has the beneficial effects that: the upper portion of retort sets up the baffle, forms the collecting tank, on the jar wall of retort, be close to the bottom of collecting tank sets up a plurality of long banding overflow mouths, the overflow mouth winds the circumference at retort jar wall place distributes, and the cambered surface distance between two adjacent overflow mouths is not more than 15. Nitric acid is fed from the lower part of the reaction tank and reacts with stone which enters the reaction tank in advance to generate calcium nitrate solution. When the liquid level of the calcium nitrate solution rises to the bottom end of the overflow port, the calcium nitrate solution overflows from the overflow port into the liquid collecting tank and is discharged from the calcium nitrate discharging pipe fitting. Because the overflow mouth is rectangular form, calcium nitrate solution by the bottom overflow of overflow mouth gets into in the collecting tank, on the one hand, impurity such as building stones of big granule is held back in the retort, realizes continuous production, and on the other hand, impurity of small granule is difficult to overflow mouth department deposit, even the deposit, along with the rising of liquid level, the overflow mouth still can keep normal ejection of compact, effectively avoids the discharge gate to be blockked up, influences normal ejection of compact, causes the tank fault accident. More importantly, the calcium nitrate solution is discharged from the periphery of the upper part of the reaction tank, so that the calcium nitrate solution is prevented from being discharged from a single outlet to cause easy formation of an inherent liquid channel, the reaction efficiency is reduced, and the nitric acid is wasted.
Drawings
Fig. 1 is a front view of a calcium nitrate reaction apparatus.
Fig. 2 is a side view of the calcium nitrate reaction apparatus.
Fig. 3 is a schematic sectional view taken along line a-a of fig. 2.
Fig. 4 is a schematic sectional view taken along line B-B in fig. 2.
In the figure: the device comprises a calcium nitrate reaction device 10, a reaction tank 100, a liquid collecting tank 110, a calcium nitrate discharging pipe 120, an overflow port 130, a stone material feeding pipe 140, a gas phase discharging pipe 150, a nitric acid feeding distributor 160, a nitric acid distributing hole 161, a solid-liquid boundary position detecting assembly 200, a heavy hammer 210, a winch 220, a locking piece 221, a steering pulley block 230, a fixed pulley 231, a pulley mounting seat 232, a traction rope 240, a dial 250, an indicating needle 260 and a baffle 300.
Detailed Description
The technical scheme and the technical effect of the invention are further elaborated in the following by combining the drawings of the invention.
Referring to fig. 1 to 3, in one embodiment, a calcium nitrate reaction apparatus 10 contacts and reacts stone and nitric acid in the calcium nitrate reaction apparatus 10 to generate a calcium nitrate solution. The calcium nitrate reaction device 10 comprises a reaction tank 100, a baffle 300 is arranged on the upper part of the reaction tank 100 close to the tank top, the baffle 300 and the outer wall of the reaction tank 100 surround to form a liquid collecting tank 110, and a calcium nitrate discharging pipe fitting 120 is arranged at the bottom of the liquid collecting tank 110. A plurality of overflow ports 130 are formed in the wall of the reaction tank 100 and close to the bottom of the liquid collecting tank 110, and the overflow ports 130 are distributed around the circumference of the wall of the reaction tank 100. The overflow outlet 130 is long and has a height greater than a width. The arc-shaped distance between two adjacent overflow ports 130 is not more than 15 degrees.
For example, the overflow outlets 130 are evenly distributed around the circumference of the reactor tank 100 where the tank wall is located, and the long sides are parallel to the axis of the reactor tank 100 or slightly skewed to both sides. The height of the overflow outlet 130 is not limited in principle, but it is desirable to ensure that the overflow outlet 130 is unobstructed and not easily blocked, preferably the height of the overflow outlet is not less than 5cm, and the maximum height of the overflow outlet should not exceed the height of the sump 110. In order to prevent impurities such as large stones from being discharged from the overflow opening 130, the width of the overflow opening 130 is not excessively large, and preferably, the width of the overflow opening 130 is 0.5cm to 1.0 cm.
The arc surface distance between two adjacent overflow ports 130 should not be undersize, and the undersize then the discharge capacity is too big, and building stones and nitric acid reaction dwell time are shorter, are unfavorable for improving nitric acid reaction efficiency. The overflow port 130 is not too large, and an inherent liquid channel is easily formed in the stone material due to the oversize, so that the contact area of the nitric acid and the stone material is reduced, and the reaction efficiency of the nitric acid is not improved. Preferably, the arc-shaped distance between two adjacent overflow ports 130 is 5 to 10 °. It should be noted that the overflow ports 130 may be uniformly distributed, or may be non-uniformly distributed within a certain range, and there is no significant difference in the improvement of the reaction efficiency of the nitric acid.
The overflow port 130 may be regular rectangle, or irregular shape, such as arc-shaped lower end face, trapezoid with shorter lower end, or triangle with upper bottom edge.
In this embodiment, nitric acid is fed from a lower portion of the reaction tank 100, and reacts with stones previously introduced into the reaction tank 100 to generate a calcium nitrate solution. When the level of the calcium nitrate solution rises to the bottom end of the overflow port 130, the calcium nitrate solution overflows from the overflow port 130 into the liquid collecting tank 110 and is discharged from the calcium nitrate discharge pipe 120. Because overflow mouth 130 is rectangular form, calcium nitrate solution by the bottom overflow of overflow mouth 130 gets into in the collecting tank 110, on the one hand, impurity such as the building stones of large granule is held back in retort 100, realizes continuous production, and on the other hand, the impurity of small granule is difficult to be in overflow mouth 130 department deposit, even the deposit, along with the rising of liquid level, the overflow mouth still can keep normal ejection of compact to wash away the impurity of deposit, effectively avoid overflow mouth 130 is blockked up, influences normal ejection of compact, causes the tank overflow accident. More importantly, the calcium nitrate solution is discharged from the periphery of the upper part of the reaction tank 100, so that the calcium nitrate solution is prevented from being discharged from a single outlet to cause easy formation of an inherent liquid channel, the reaction efficiency is reduced, and the nitric acid is wasted. Experiments show that the calcium nitrate solution is prepared by adopting the calcium nitrate reaction device designed by the invention, and the content of nitric acid in a sample obtained by sampling the calcium nitrate discharging pipe fitting 120 is reduced by 30-50% compared with that of a reaction device with a single outlet, so that the reaction efficiency of nitric acid is greatly improved, and the dosage of nitric acid is reduced.
Referring to fig. 4, in one embodiment, the reaction tank 100 is provided with a stone material feeding pipe 140 and a gas phase discharging pipe 150 at the top and a nitric acid feeding distributor 160 at the bottom. The stone material feeding pipe 140 is used for introducing stone material into the reaction tank 100, and the gas phase discharging pipe 150 is used for collecting CO generated in the contact reaction process of the stone material and nitric acid2Waiting for gas, and performing centralized treatment and discharge. The nitric acid feed distributor 160 is used for introducing nitric acid into the reaction tank 100 from the bottom of the reaction tank 100. Preferably, the nitric acid feed distributor 160 is cross-shaped to facilitate uniform feeding, reduce pressure of the rock material on the nitric acid feed distributor 160, and extend the nitric acid feed distributionThe service life of the device 160. A plurality of nitric acid distributing holes 161 are formed below the nitric acid feeding distributor 160, so that the nitric acid feeding is smoother, and small particle impurities are prevented from entering the nitric acid feeding distributor 160 to cause blockage.
In a preferred embodiment, the reaction tank 100 is further provided with a solid-liquid boundary position detecting assembly 200, the solid-liquid boundary position detecting assembly 200 includes a weight 210, a winch 220, a steering pulley block 230 and a traction rope 240, the weight 210 is disposed in the reaction tank 100, the winch 220 is mounted on the outer wall of the reaction tank 100, the steering pulley block 230 is fixed on the tank top of the reaction tank 100, one end of the traction rope 240 is connected to the weight 210, and the other end of the traction rope passes through the tank top of the reaction tank 100, is erected on the steering pulley block 230, and is wound on the winch 220. The winch 220 is rotated, and the traction rope 240 can be wound on the winch 220 or released from the winch 220, so that the weight 210 is lifted in a vertical direction.
The solid-liquid boundary position detection assembly 200 comprising a heavy hammer 210, a winch 220, a steering pulley block 230 and a traction rope 240 is arranged on the reaction tank 100, the winch 220 is rotated to release the traction rope 240 in the contact reaction process of stone and calcium nitrate, the heavy hammer 210 descends along the vertical direction under the steering action of the steering pulley block 230 until the lower surface of the heavy hammer 210 is in contact with the surface of the stone, the heavy hammer 210 stops descending, and at the moment, the stone level in the reaction tank 100 can be visually acquired through the displacement of the traction rope 240 relative to the winch 220. As the stone material level descends along with the reaction, the weight 210 descends along with the stone material level, tracks and detects the current stone material level, monitors the reaction process, and provides effective data support for selection of stone material replenishment opportunity. Secondly, solid-liquid boundary position detection subassembly 200 simple structure measures accurately, and is not fragile, compares that current level gauge or charge level indicator have unique advantage.
In one embodiment, in order to facilitate visual observation of the boundary position between the rock and the calcium nitrate solution, a dial 250 is disposed on the outer wall of the reaction tank 100, an indicator needle 260 is disposed at one end of the traction rope 240 close to the winch 220, and an orthographic projection of the indicator needle 260 can coincide with the dial 250. For example, when the reaction tank 100 is filled with stone, the winch 220 is rotated to wind the traction rope 240 around the winch 220 and the weight 210 is located at the highest point, and at this time, the orthographic projection of the pointer 260 is located at the lower end of the scale plate 250, i.e., at the highest point of the solid-liquid separation position. After the stone filling is completed, the weight 210 is naturally dropped, and the pointer 260 moves upward. When the weight 210 contacts the solid-liquid boundary position, the weight stops falling, and at this time, the displacement of the pulling rope 240 relative to the capstan 220, that is, the relative displacement of the pointer 260, is the current solid-liquid boundary position. As the solid-liquid reaction proceeds, the stone is consumed, the solid-liquid boundary position moves downward, the weight 210 moves downward, and the pointer 260 moves upward to obtain the solid-liquid boundary position in the reaction process in real time.
In a preferred embodiment, the diverting pulley assembly 230 includes at least one fixed pulley 231 and a pulley mounting seat 232 arranged side by side, the pulley mounting seat 232 is fixed on the tank top of the reaction tank 100, and the fixed pulley 231 is mounted in the pulley mounting seat 232. The traction rope 240 passes around the fixed pulley 231, so that the traction rope 240 is prevented from contacting the wall of the reaction tank 100, the wear of the traction rope 240 is reduced, the service life of the traction rope 240 is prolonged, and the installation position of the heavy hammer 210 can be as close as possible to the middle of the reaction tank 100 by using the steering pulley block 230, so that the measurement is more accurate.
In one embodiment, the area of the lower surface of the weight 210 is not less than 50cm2So that the heavy punch 210 can be stably contacted with the upper surface of the stone, the measurement error caused by local protrusion or depression of the upper surface of the stone is reduced, and the accuracy of the measurement of the solid-liquid boundary position is improved.
In another embodiment, a lock 221 is disposed on the winch 220, and in the measuring state, the lock 221 is opened, and the winch 220 rotates to enable the weight 210 to fall normally. When the stone is fed, the weight 210 is lifted to the highest point, and the winch 220 is locked by the locking piece 221, so that the weight 210 is prevented from being pressed to the bottom of the stone in the stone feeding process.
Further, a return member is disposed on the winch 220, and the return member provides a return force to allow the pulling rope 240 to wind on the winch 220. The restoring force provided by the restoring member is smaller than the difference between the gravity of the weight 210 and the buoyancy of the weight 210 in the calcium nitrate solution.
The technical effects of the present invention will be further described below by specific experimental examples.
Comparative example 1
The reaction tank 100 is arranged, and the volume is 200m3And a calcium nitrate discharging pipe 120, a stone feeding pipe 140, a gas phase discharging pipe 150 and a nitric acid feeding distributor 160 are arranged on the reaction tank. The method comprises the steps of filling 2/3-volume stones (the stone grain size is about 1 cm-3 cm) into a reaction tank 100, adding nitric acid with the mass concentration of 40% into the reaction tank 100 through a nitric acid feeding distributor 160, carrying out reaction for a period of time, and detecting the nitric acid concentration of discharged materials at a calcium nitrate discharging pipe fitting 120 after the discharged materials are stable. The concentration of nitric acid in the calcium nitrate solution is 2-15%.
Comparative example No. two
The reaction tank 100 is arranged, and the volume is 200m3And on the reaction tank 100 are a stone feeding pipe 140, a gas phase discharging pipe 150 and a nitric acid feeding distributor 160. An annular liquid outlet bin is fixed on the outer wall of the reaction tank 100 and communicated with the reaction bin through a flange port, the flange port is arranged at the lower part of the annular liquid outlet bin, and a reaction liquid discharge port is arranged at the upper part of the annular liquid outlet bin. The flange opening is obliquely fixed with a baffle, and the baffle and the flange opening form a clamping opening. The method comprises the steps of filling 2/3-volume stones (the stone grain size is about 1 cm-3 cm) into a reaction tank 100, adding nitric acid with the mass concentration of 40% into the reaction tank 100 through a nitric acid feeding distributor 160, carrying out reaction for a period of time, and detecting the nitric acid concentration of discharged materials at a calcium nitrate discharging pipe fitting 120 after the discharged materials are stable. The concentration of nitric acid in the calcium nitrate solution is 2-15%.
Experimental example 1
The reaction tank 100 is arranged, and the volume is 200m3And is fed into the reaction tank 100A material pipe 140, a gas phase discharging pipe 150 and a nitric acid feeding distributor 160. The outer wall of the reaction tank 100 is provided with a liquid collecting groove 110, and the bottom of the liquid collecting groove 110 is provided with a calcium nitrate discharging pipe fitting 120. On the wall of the reaction tank 100, 4 overflow ports 130 are opened at the bottom close to the liquid collecting tank 110, and the overflow ports 130 are distributed around the circumference of the wall of the reaction tank 100. The overflow outlet 130 is long and has a height greater than a width. The method comprises the steps of filling 2/3-volume stones (the stone grain size is about 1 cm-3 cm) into a reaction tank 100, adding nitric acid with the mass concentration of 40% into the reaction tank 100 through a nitric acid feeding distributor 160, carrying out reaction for a period of time, and detecting the nitric acid concentration of discharged materials at a calcium nitrate discharging pipe fitting 120 after the discharged materials are stable. The concentration of nitric acid in the calcium nitrate solution is 2-15%.
Experimental example two
The number of overflow ports 130 in the first experimental example was increased to 24, and the other conditions were not changed. The concentration of the nitric acid in the calcium nitrate solution is detected to be 2-10%.
Experimental example III
The number of overflow ports 130 in the second experimental example was increased to 36, and the other conditions were not changed. The concentration of the nitric acid in the calcium nitrate solution is detected to be 2-7%.
Experimental example four
The number of overflow ports 130 in the second experimental example was increased to 72, and the other conditions were not changed. The concentration of the nitric acid in the calcium nitrate solution is detected to be 2-12%.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (9)
1. A calcium nitrate reaction device comprises a reaction tank and is characterized in that a baffle is arranged on the upper portion of the reaction tank close to the top of the reaction tank, a liquid collecting tank is formed by the baffle and the outer wall of the reaction tank in a surrounding mode, and a calcium nitrate discharging pipe fitting is arranged at the bottom of the liquid collecting tank;
a plurality of overflow ports are formed in the tank wall of the reaction tank and close to the bottom of the liquid collecting tank, the overflow ports are distributed around the circumference of the tank wall of the reaction tank, and the overflow ports are long-strip-shaped and have the height larger than the width; the arc surface distance between two adjacent overflow ports is not more than 15 degrees, and the width of each overflow port is 0.5 cm-1.0 cm.
2. The calcium nitrate reaction device according to claim 1, wherein the arc distance between two adjacent overflow ports is 5 ° to 10 °.
3. The calcium nitrate reaction device as claimed in claim 1, wherein the reaction tank is provided with a stone feeding pipe and a gas phase discharging pipe at the top and a nitric acid feeding distributor at the bottom.
4. The calcium nitrate reaction device as claimed in claim 4, wherein the nitric acid feeding distributor is cross-shaped, and a plurality of nitric acid distributing holes are formed below the nitric acid feeding distributor.
5. The calcium nitrate reaction device according to any one of claims 1 to 4, wherein a solid-liquid boundary position detecting component is further provided on the reaction tank, the solid-liquid boundary position detecting component comprises a heavy hammer, a winch, a steering pulley block and a traction rope, the heavy hammer is provided in the reaction tank, the winch is mounted on the outer wall of the reaction tank, the steering pulley block is fixed on the tank top of the reaction tank, one end of the traction rope is connected with the heavy hammer, the other end of the traction rope passes through the tank top of the reaction tank, is erected on the steering pulley block, and is wound on the winch; the winch rotates, and the traction rope can be wound on or released from the winch so as to lift the heavy hammer in the vertical direction.
6. The calcium nitrate reaction device according to claim 5, wherein a dial is provided on the outer wall of the reaction tank, and an indicator needle is provided at an end of the pulling rope near the capstan, and an orthographic projection of the indicator needle can coincide with the dial.
7. The calcium nitrate reaction device according to claim 5, wherein the diverting pulley set comprises at least one fixed pulley arranged side by side and a pulley mounting seat fixed on the top of the reaction tank, the fixed pulley being mounted in the pulley mounting seat.
8. The calcium nitrate reaction device of claim 5 wherein the area of the lower surface of the weight is not less than 50cm2。
9. The calcium nitrate reaction device according to claim 5, wherein a locking member is provided on the winch.
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| CN202110068712.7A CN112934118B (en) | 2021-01-19 | 2021-01-19 | Calcium nitrate reaction device |
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Cited By (1)
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| CN112939632A (en) * | 2021-01-19 | 2021-06-11 | 宁夏润安微肥科技有限公司 | Calcium ammonium nitrate production system |
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