CN109399569B - Method for preparing hydrogen chloride by sulfuric acid extraction method - Google Patents
Method for preparing hydrogen chloride by sulfuric acid extraction method Download PDFInfo
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- CN109399569B CN109399569B CN201811627074.2A CN201811627074A CN109399569B CN 109399569 B CN109399569 B CN 109399569B CN 201811627074 A CN201811627074 A CN 201811627074A CN 109399569 B CN109399569 B CN 109399569B
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- C01B7/00—Halogens; Halogen acids
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- C01B7/0706—Purification ; Separation of hydrogen chloride
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Abstract
The invention belongs to the technical field of hydrogen chloride preparation, and particularly relates to a method for preparing hydrogen chloride by a sulfuric acid extraction method; the hydrogen chloride preparation device used in the method comprises a reaction chamber, a sulfuric acid spray nozzle fixed on the upper part of the reaction chamber, a hydrochloric acid guide pipe penetrating into the center of the lower end of the reaction chamber from bottom to top, a hydrochloric acid spray nozzle, a mixing module and a power module; the upper end of the reaction chamber is provided with an air outlet, the center of the lower end of the reaction chamber is provided with a discharge port, and the side wall of one side of the reaction chamber is provided with a square cavity; the hydrochloric acid spray head is arranged at the upper end of the hydrochloric acid guide pipe and is positioned at the lower end of the sulfuric acid spray head; the mixing module comprises a sliding sleeve and a stepped sliding extrusion strip; the power module comprises a power lead screw and a first sliding block; the invention can accelerate the mixing degree of concentrated sulfuric acid and concentrated hydrochloric acid through the mixing module, and can ensure that the concentrated sulfuric acid fully dehydrates the concentrated hydrochloric acid, thereby preparing high-quality hydrogen chloride gas with high purity and less water content.
Description
Technical Field
The invention belongs to the technical field of hydrogen chloride preparation, and particularly relates to a method for preparing hydrogen chloride by a sulfuric acid extraction method.
Background
In the prior art, hydrogen chloride gas is an important raw material for producing chlorosulfonic acid in a sulfuric acid plant, the sulfuric acid plant does not have the hydrogen chloride gas and must be transported from other chlor-alkali plants, but the hydrogen chloride gas can be directly transported by a pipeline unless the plants are very close to the sulfuric acid plant, and the hydrogen chloride gas is only produced by a thermal desorption method after the hydrochloric acid is transported to the sulfuric acid plant. However, since the constant boiling point concentration of hydrochloric acid is 20.2%, when the hydrochloric acid concentration is resolved from 30% to a concentration close to the constant boiling point concentration of 21% -23% by a general "heat desorption method", the precipitation of pure hydrogen chloride gas is stopped, so that the utilization rate of the hydrogen chloride precipitated from the hydrochloric acid is extremely low, a large amount of 21% -23% light hydrochloric acid cannot be used in a sulfuric acid plant, and only a large amount of manpower and material resources are consumed, the light hydrochloric acid returns to a chlor-alkali plant to reabsorb the hydrogen chloride to prepare 30% of finished hydrochloric acid. This is a costly return trip.
Some technical solutions of hydrogen chloride production equipment have appeared in the prior art, and for example, a chinese patent with application number 932371701 discloses a hydrogen chloride generator for a sulfuric acid extraction method, which includes a tower-shaped barrel body, a concentrated sulfuric acid and hydrochloric acid spray pipe, a hydrogen chloride gas outlet and a dilute sulfuric acid discharge pipe.
The generator in the technical scheme utilizes the strong dehydration property of concentrated sulfuric acid to prepare hydrogen chloride gas from hydrochloric acid, thereby greatly improving the utilization rate of the hydrochloric acid, reducing transportation and lowering cost. The hydrogen chloride obtained by the generator has high purity, is dry, has higher purity than the hydrogen chloride gas synthesized by a common chlor-alkali plant, and has less water. And saves energy sources compared with the common method of preparing hydrogen chloride by adopting a thermal desorption method. It does not require a heat source at all. And also release heat energy. However, in such hydrogen chloride production equipment, the mixed solution is not stirred when the concentrated sulfuric acid and the hydrochloric acid are mixed, so that the dehydration effect of the concentrated sulfuric acid is reduced, the generation amount of hydrogen chloride gas is reduced, hydrochloric acid remains in the mixed solution, waste is caused, and the cost is increased; meanwhile, the prepared hydrogen chloride is stored in the storage tank, and due to the air tightness problem, a small amount of hydrogen chloride overflows from the storage tank, so that potential safety hazards are caused.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention provides a method for preparing hydrogen chloride by a sulfuric acid extraction method, and aims to safely prepare high-quality hydrogen chloride gas with high purity and less water.
The technical scheme adopted by the invention for solving the technical problems is as follows: the invention relates to a method for preparing hydrogen chloride by a sulfuric acid extraction method, which comprises the following steps:
s1, introducing concentrated hydrochloric acid into a hydrochloric acid conduit in the hydrogen chloride preparation device, introducing concentrated sulfuric acid into a sulfuric acid spray head in the hydrogen chloride preparation device, and preparing hydrogen chloride by using the hydrogen chloride preparation device;
s2, communicating the gas outlet of the hydrogen chloride preparation device in the S1 with two liquid storage tanks which are connected in series and are both filled with concentrated sulfuric acid, and sequentially filling hydrogen chloride into the two liquid storage tanks which are filled with concentrated sulfuric acid for drying;
s3, storing the collected hydrogen chloride gas in the storage tank for three to five minutes after the hydrogen chloride is prepared in S2; other gases are mixed in the hydrogen chloride which is just prepared, so that the purity of the hydrogen chloride gas is not high, and the hydrogen chloride gas with low purity is removed;
s4, sleeving a sealing bag with a slaked lime layer on the storage tank at S3, sealing the storage tank for collecting the hydrogen chloride by using the sealing bag, and reacting the slaked lime with the overflowed hydrogen chloride to avoid the overflowed hydrogen chloride gas from corroding surrounding articles or causing harm to human bodies and realize the safe collection of the hydrogen chloride;
the hydrogen chloride preparation devices in the S1 and S2 comprise a reaction chamber, a sulfuric acid spray nozzle fixed on the upper part of the reaction chamber, a hydrochloric acid guide pipe penetrating into the center of the lower end of the reaction chamber from bottom to top, a hydrochloric acid spray nozzle, a mixing module and a power module; the upper end of the reaction chamber is provided with an air outlet for collecting hydrogen chloride gas, one side of the lower end of the reaction chamber is provided with a discharge port for discharging dilute sulfuric acid, and the side wall of one side of the reaction chamber is provided with a square cavity; the hydrochloric acid spray head is arranged at the upper end of the hydrochloric acid guide pipe, and the hydrochloric acid spray head is positioned at the lower end of the sulfuric acid spray head; the mixing module comprises a sliding sleeve and a stepped sliding extrusion strip; the sliding sleeve is sleeved on the hydrochloric acid guide pipe and is in sliding connection with the hydrochloric acid guide pipe, and the sliding sleeve is a magnet; one end of the sliding extrusion strip is hinged with the sliding sleeve, the other end of the sliding extrusion strip is hinged with the side wall of the reaction chamber, and at least four sliding extrusion strips are arranged around the rotation center of the sliding sleeve; the sliding extrusion strip comprises a plurality of strip-shaped sliding blocks and pull ropes; the strip-shaped sliding blocks are provided with sliding grooves, adjacent strip-shaped sliding blocks are connected in a sliding mode through the sliding grooves and are arranged in a stepped mode, one strip-shaped sliding block located at the end is hinged to the square sliding strip, and the other strip-shaped sliding block located at the end is hinged to the side wall of the reaction chamber; the pull rope is used for connecting two adjacent strip-shaped sliding blocks, so that the two adjacent strip-shaped sliding blocks are prevented from sliding and separating; the power module comprises a power lead screw and a first sliding block; the power screw rod and the first sliding block are arranged at the square cavity of the side wall of the reaction chamber; the first sliding block is in sliding fit with the square cavity and is a magnet; the power lead screw penetrates through the first sliding block, the first sliding block is driven by the forward and reverse rotation of the power lead screw to slide back and forth in the square cavity to attract the sliding sleeve to slide along with the sliding, and the strip-shaped sliding blocks hinged with the sliding sleeve are pulled or pressed to cause the adjacent strip-shaped sliding blocks to slide. When the device works, concentrated sulfuric acid is downwards sprayed out from a sulfuric acid spray head, concentrated hydrochloric acid is guided in through a hydrochloric acid guide pipe and then is sprayed out from a hydrochloric acid spray head, the concentrated sulfuric acid is mixed with the concentrated hydrochloric acid, the concentrated sulfuric acid is used for continuously extracting water in the hydrochloric acid and continuously releasing heat, so that chlorine hydride in the hydrochloric acid is absorbed and escaped, the hydrogen chloride gas is in countercurrent contact with the concentrated sulfuric acid which is continuously sprayed when rising, the hydrogen chloride gas is fully dried, high-quality hydrogen chloride gas with high purity and less water is obtained from a gas outlet, and the dilute sulfuric acid is discharged from a discharge port; specifically, when the power screw rotates forwards and backwards, the first sliding block slides back and forth in the square cavity, the first sliding block enables the suction sliding sleeve to slide back and forth on the hydrochloric acid guide pipe, and the first sliding block enables the suction sliding sleeve to slide along with the suction sliding sleeve, so that the strip-shaped sliding blocks hinged with the sliding sleeves are pulled or pressed to cause the adjacent strip-shaped sliding blocks to slide; after concentrated sulfuric acid and concentrated hydrochloric acid mix the spout that falls on the bar slider in, adjacent bar slider slides and is close to, will make two bar sliders extrude the mixture of concentrated sulfuric acid and concentrated hydrochloric acid in the spout jointly, under the slip striking between two adjacent bar sliders, concentrated sulfuric acid and concentrated hydrochloric acid in the spout are hit and are flown the mixing dispersion, thereby effectively promote the continuous moisture in the extraction concentrated hydrochloric acid of concentrated sulfuric acid, and release the heat constantly, thereby make hydrogen chloride in the hydrochloric acid flee by the desorption, the hydrogen chloride that spills over is discharged from the gas outlet, realize dry hydrogen chloride and collect.
Furthermore, a blind hole is horizontally formed in the upper part of one side of the strip-shaped sliding block; the blind hole is internally provided with an air-through block and a reset spring, and the upper end of the middle part of the blind hole is provided with a through hole communicated with the outside of the strip-shaped sliding block; the ventilation block is provided with a right-angle hole, and the ventilation block slides in the blind hole to the through hole to communicate the inside of the sliding chute with the through hole; the reset spring is connected with the inner wall of the blind hole and the ventilation block; a guide plate which is flush with the upper end of the sliding chute is arranged on the inner side wall of the sliding chute; the baffle gets into the blind hole extrusion piece of ventilating and makes the piece of ventilating move to through-hole department when two adjacent bar sliders are close to, and the spout is in the encapsulated situation after the baffle gets into in the blind hole, and concentrated sulfuric acid and concentrated hydrochloric acid mixture in the spout will last to be pressed to the spout and release after the through-hole intercommunication. The during operation, in the in-process that two adjacent bar sliders closed together, the baffle will get into in the blind hole and promote the piece of ventilating and slide in the blind hole, make the piece of ventilating communicate through-hole and spout when reaching through-hole department, and get into the blind hole at the baffle and when the piece of ventilating did not reach through-hole department, the spout is in the encapsulated situation, concentrated sulfuric acid and concentrated hydrochloric acid mixture in the spout will be compressed, behind piece intercommunication through-hole and the spout of ventilating, the concentrated sulfuric acid and the concentrated hydrochloric acid that compress in the spout will be extruded in the twinkling of an eye away, thereby make the abundant mixture of concentrated sulfuric acid and concentrated hydrochloric acid and make the concentrated hydrochloric acid dehydrated, hydrogen chloride among the concentrated hydrochloric acid spills over, make the hydrogen chloride gasification rate among the concentrated hydrochloric acid improve, and hydrogen chloride still can be continued to dewater by the concentrated sulfuric acid that drenches from above, make hydrogen chloride dry, thereby obtain the high.
Furthermore, two threads with opposite rotation directions are arranged on the surface of the power screw rod; the two sets of the mixing modules are arranged, the mixing modules on the upper portion of the hydrochloric acid guide pipe and the mixing modules on the lower portion of the hydrochloric acid guide pipe are symmetrically arranged, the first sliding blocks in the power modules are respectively located at two threads on the power screw rod, and the power screw rod rotates to enable the first sliding blocks on the power screw rod to slide away from or towards each other. The during operation, when the mixed module of hydrochloric acid pipe lower extreme is walked over to partly concentrated sulfuric acid and concentrated hydrochloric acid mixture, the mixture of concentrated sulfuric acid and concentrated hydrochloric acid fills in the spout of bar slider, draw close the mixture that will extrude concentrated sulfuric acid and concentrated hydrochloric acid between the adjacent bar slider, make pressurized concentrated sulfuric acid and concentrated hydrochloric acid will be extruded in the twinkling of an eye and go out, thereby make the abundant mixing of concentrated sulfuric acid and concentrated hydrochloric acid and make concentrated hydrochloric acid be dehydrated, hydrogen chloride in the concentrated hydrochloric acid spills over, the hydrogen chloride rate of gasification among the concentrated hydrochloric acid improves, and hydrogen chloride still can be continued the dehydration by the concentrated sulfuric acid that drenches from the top, make hydrogen chloride by the drying, thereby obtain the high-quality hydrogen chloride gas that purity is high, the moisture.
Further, a sleeve is fixedly arranged at the upper end of the through hole in the strip-shaped sliding block; the upper end of the sleeve is rotatably connected with a cake block, and the sleeve is communicated with the through hole; a plurality of liquid outlet holes are formed in the round cake block; and one end of each liquid outlet hole is communicated with the sleeve, and the other end of each liquid outlet hole is attached to the edge of the round cake block. The during operation, the back is given vent to anger from the through-hole to strong brine and concentrated sulfuric acid mixture in the spout by the extrusion, through the sleeve pipe get into in the cake piece and along going out liquid hole departure, because of the other end and the cake piece edge laminating of going out the liquid hole, thereby make to drive the cake piece rotation when strong brine and concentrated sulfuric acid spiral departure, be favorable to the intensive mixing of concentrated sulfuric acid and strong hydrochloric acid on the one hand, make the strong hydrochloric acid by the dehydration, on the other hand is favorable to the mixture separation of hydrogen chloride and strong hydrochloric acid and concentrated sulfuric acid, make the hydrogen chloride easily collected.
Further, an air outlet groove is formed at the air outlet; an air outlet block is arranged at the air outlet groove; the edge of the gas outlet block is provided with a gas outlet hole, the gas outlet block falls on the gas outlet groove under the action of self gravity to block the gas outlet, and the gas outlet block is extruded by the hydrogen chloride gas to move upwards to communicate the gas outlet and the gas outlet hole; the upper end of the power screw is provided with an impeller, and the middle part of the power screw is provided with a coil spring; an air passage is arranged above the air outlet block, and the air passage is communicated with the impeller tangentially and then communicated with the outside of the reaction chamber; the impeller rotates when the hydrogen chloride gas flows through, and the impeller is reset by the coil spring to rotate when the hydrogen chloride gas stops discharging. When the device works, after the pressure of hydrogen chloride gas in the reaction chamber is increased, the hydrogen chloride gas pushes the gas outlet block to move upwards, the gas outlet hole is communicated with the reaction chamber and the air passage after the gas outlet block moves upwards, and the hydrogen chloride gas impacts the impeller to enable the power screw rod to rotate, so that the power screw rod has power without being driven by a motor, on one hand, electric energy is saved, and on the other hand, the manufacturing cost of the device is reduced; and after hydrogen chloride spills over from the piece of giving vent to anger, hydrogen chloride gas pressure in the reaction chamber reduces, the piece of giving vent to anger is under self action of gravity and whereabouts shutoff gas outlet, make hydrogen chloride gas short-lived stop blowing to the impeller again, thereby make the power lead screw short-lived the power source that loses, thereby make the wind spring will make the power lead screw reversal when reseing, No. two sliders on the power lead screw will return, make two adjacent bar sliders slide and keep away from, wait for hydrogen chloride gas pressure in the reaction chamber to urge the power lead screw to rotate after an increase, under concentrated hydrochloric acid and concentrated sulfuric acid constantly let in the condition, realize the preparation of hydrogen chloride continuously.
Further, an elastic scraping blade is arranged at the orifice of the blind hole; the upper end of the guide plate is provided with an arc-shaped groove, and when the guide plate enters the blind hole, the surface of the arc-shaped groove on the guide plate is scraped by the elastic scraper. The during operation, concentrated sulfuric acid and concentrated sulfuric acid spray behind down, part concentrated sulfuric acid and concentrated hydrochloric acid mixture will spill on the arc recess on the baffle, make the arc recess on accumulate to have concentrated sulfuric acid and concentrated hydrochloric acid mixture, the in-process that gets into the blind hole at the baffle, elastic scraping blade on the blind hole will accumulate to have concentrated sulfuric acid and concentrated hydrochloric acid mixture to save on the arc recess and collapse to fly, thereby promote the abundant mixture of concentrated sulfuric acid and concentrated hydrochloric acid and make concentrated hydrochloric acid by the dehydration, hydrogen chloride among the concentrated hydrochloric acid spills over, make the hydrogen chloride rate of gasification among the concentrated hydrochloric acid improve, and hydrogen chloride still can be continued the dehydration by the concentrated sulfuric acid that drenches from the top, make hydrogen chloride by the drying, thereby obtain the high-quality hydrogen chloride gas that purity is high, the moisture is.
The invention has the following beneficial effects:
1. according to the invention, the hydrogen chloride gas is dried by the two liquid storage tanks connected in series, and the high-quality hydrogen chloride gas with high purity and less moisture is prepared by removing other impurity gases in the reaction chamber; the sealing bag with the slaked lime layer is sleeved on the outer layer of the storage tank, the storage tank for collecting the hydrogen chloride is sealed by the sealing bag, and the slaked lime and the overflowed hydrogen chloride are subjected to neutralization reaction, so that the overflowed hydrogen chloride gas is prevented from corroding surrounding articles or causing harm to human bodies, and the safe collection of the hydrogen chloride is realized.
2. The invention has simple structure, can accelerate the mixing degree of concentrated sulfuric acid and concentrated hydrochloric acid through the mixing module, can ensure that the concentrated sulfuric acid fully dehydrates the concentrated hydrochloric acid, and the prepared hydrogen chloride gas is dried again through the concentrated sulfuric acid from top to bottom, thereby preparing high-quality hydrogen chloride gas with high purity and less moisture, and improving the conversion rate of converting the concentrated sulfuric acid into the hydrogen chloride gas.
3. The method utilizes the strong dehydration property of concentrated sulfuric acid to prepare hydrogen chloride gas from hydrochloric acid, greatly improves the utilization rate of the hydrochloric acid, reduces transportation and reduces cost; the hydrogen chloride obtained by the method has high purity, is dry, has higher purity than the hydrogen chloride gas synthesized by a common chlor-alkali plant, and has less water; the method for preparing hydrogen chloride gas saves energy sources compared with the commonly adopted 'heat desorption method', does not need a heat source at all, and can release heat energy.
Drawings
FIG. 1 is a flow chart of a method of the present invention;
FIG. 2 is a schematic view of the hydrogen chloride production apparatus of the present invention;
FIG. 3 is a connection diagram of two adjacent bar-shaped sliders according to the present invention;
FIG. 4 is a cross-sectional view taken about A-A in FIG. 3;
in the figure: the device comprises a reaction chamber 1, an air outlet 11, a discharge port 12, a sulfuric acid spray nozzle 13, a hydrochloric acid guide pipe 14, a hydrochloric acid spray nozzle 15, a square cavity 16, a mixing module 2, a sliding sleeve 21, a strip-shaped sliding block 3, a sliding groove 31, a ventilation block 32, a return spring, a through hole 33, a guide plate 34, a round cake block 35, a liquid outlet hole 351, a blind hole 36, a power module 4, a power screw 41, a first sliding block 42, an air outlet groove 43, an air outlet block 44, an impeller 45, a coil spring 46, an air passage 47, an elastic scraper 48 and an arc-shaped.
Detailed Description
The method for producing hydrogen chloride by the sulfuric acid extraction method according to the present invention is described below with reference to fig. 1 to 4.
As shown in fig. 1 to 4, the method for preparing hydrogen chloride by using a sulfuric acid extraction method according to the present invention comprises the following steps:
s1, introducing concentrated hydrochloric acid into a hydrochloric acid conduit in the hydrogen chloride preparation device, introducing concentrated sulfuric acid into a sulfuric acid spray head in the hydrogen chloride preparation device, and preparing hydrogen chloride by using the hydrogen chloride preparation device;
s2, communicating the gas outlet of the hydrogen chloride preparation device in the S1 with two liquid storage tanks which are connected in series and are both filled with concentrated sulfuric acid, and sequentially filling hydrogen chloride into the two liquid storage tanks which are filled with concentrated sulfuric acid for drying;
s3, storing the collected hydrogen chloride gas in the storage tank for three to five minutes after the hydrogen chloride is prepared in S2; other gases are mixed in the hydrogen chloride which is just prepared, so that the purity of the hydrogen chloride gas is not high, and the hydrogen chloride gas with low purity is removed;
s4, sleeving a sealing bag with a slaked lime layer on the storage tank at S3, sealing the storage tank for collecting the hydrogen chloride by using the sealing bag, and reacting the slaked lime with the overflowed hydrogen chloride to avoid the overflowed hydrogen chloride gas from corroding surrounding articles or causing harm to human bodies and realize the safe collection of the hydrogen chloride;
the hydrogen chloride preparation devices in the S1 and S2 comprise a reaction chamber 1, a sulfuric acid spray nozzle 13 fixed at the upper part of the reaction chamber 1, a hydrochloric acid guide pipe 14 penetrating into the center of the lower end of the reaction chamber 1 from bottom to top, a hydrochloric acid spray nozzle 15, a mixing module 2 and a power module 4; the upper end of the reaction chamber 1 is provided with an air outlet 11 for collecting hydrogen chloride gas, one side of the lower end of the reaction chamber 1 is provided with a discharge port 12 for discharging dilute sulfuric acid, and the side wall of one side of the reaction chamber 1 is provided with a square cavity 16; the hydrochloric acid spray head 15 is arranged at the upper end of the hydrochloric acid guide pipe 14, and the hydrochloric acid spray head 15 is positioned at the right lower end of the sulfuric acid spray head 13; the mixing module 2 comprises a sliding sleeve 21 and a stepped sliding extrusion strip; the sliding sleeve 21 is sleeved on the hydrochloric acid guide pipe 14, the sliding sleeve 21 is in sliding connection with the hydrochloric acid guide pipe 14, and the sliding sleeve 21 is a magnet; one end of the sliding extrusion strip is hinged with the sliding sleeve 21, the other end of the sliding extrusion strip is hinged with the side wall of the reaction chamber 1, and at least four sliding extrusion strips are arranged around the rotation center of the sliding sleeve 21; the sliding extrusion strip comprises a plurality of strip-shaped sliding blocks 3 and pull ropes; the strip-shaped sliding blocks 3 are provided with sliding grooves 31, the adjacent strip-shaped sliding blocks 3 are connected in a sliding mode through the sliding grooves 31 and are arranged in a step shape, one strip-shaped sliding block 3 positioned at the end part is hinged with the square sliding strip, and the other strip-shaped sliding block 3 positioned at the end part is hinged with the side wall of the reaction chamber 1; the pull rope is used for connecting two adjacent strip-shaped sliding blocks 3, so that the two adjacent strip-shaped sliding blocks 3 are prevented from sliding and separating; the power module 4 comprises a power screw 41 and a first sliding block 42; the power screw 41 and the first sliding block 42 are arranged at the square cavity 16 of the side wall of the reaction chamber 1; the first sliding block 42 is in sliding fit with the square cavity 16, and the first sliding block 42 is a magnet; the power screw 41 penetrates through the first sliding block 42, the power screw 41 rotates positively and negatively to drive the first sliding block 42 to slide back and forth in the square cavity 16 to attract the sliding sleeve 21 to slide along, and the strip-shaped sliding blocks 3 hinged with the sliding sleeve 21 are pulled or pressed to cause the adjacent strip-shaped sliding blocks 3 to slide. When the device works, concentrated sulfuric acid is downwards sprayed out from a sulfuric acid spray nozzle 13, the concentrated hydrochloric acid is sprayed out from a hydrochloric acid spray nozzle 15 after being guided in through a hydrochloric acid guide pipe 14, the concentrated sulfuric acid is mixed with the concentrated hydrochloric acid, the strong dehydration property of the concentrated sulfuric acid continuously extracts water in the hydrochloric acid and continuously releases heat, so that hydrogen chloride in the hydrochloric acid is absorbed and escaped, the hydrogen chloride gas is in countercurrent contact with the concentrated sulfuric acid continuously sprayed downwards when rising, the hydrogen chloride gas is fully dried, high-quality hydrogen chloride gas with high purity and less water is obtained from a gas outlet 11, and the dilute sulfuric acid is discharged from a discharge port 12; specifically, when the power screw 41 rotates forward and backward, the first sliding block 42 slides back and forth in the square cavity 16, the first sliding block 42 slides the suction sliding sleeve 21 back and forth on the hydrochloric acid conduit 14, and the first sliding block 42 slides the suction sliding sleeve 21 along with the suction sliding sleeve, so that the bar-shaped sliding blocks 3 hinged with the sliding sleeve 21 are pulled or pressed to cause the sliding between the adjacent bar-shaped sliding blocks 3; after concentrated sulfuric acid and concentrated hydrochloric acid are mixed and then fall into the chute 31 on the bar-shaped sliding block 3, the adjacent bar-shaped sliding blocks 3 slide and approach to each other, so that the two bar-shaped sliding blocks 3 jointly extrude the mixture of concentrated sulfuric acid and concentrated hydrochloric acid in the chute 31, under the sliding impact between the two adjacent bar-shaped sliding blocks 3, the concentrated sulfuric acid and the concentrated hydrochloric acid in the chute 31 are knocked to fly, mixed and dispersed, thereby effectively promoting the concentrated sulfuric acid to continuously extract moisture in the concentrated hydrochloric acid, and continuously releasing heat, thereby enabling hydrogen chloride in the hydrochloric acid to be desorbed and escaped, overflowed hydrogen chloride is discharged from the gas outlet 11, and dry hydrogen chloride collection is realized.
Further, a blind hole 36 is horizontally arranged at the upper part of one side of the strip-shaped sliding block 3; the blind hole 36 is internally provided with an air-through block 32 and a return spring, and the upper end of the middle part of the blind hole 36 is provided with a through hole 33 communicated with the outside of the strip-shaped sliding block 3; the ventilation block 32 is provided with a right-angle hole, and the ventilation block 32 slides to the through hole 33 in the blind hole 36 to communicate the inside of the sliding chute 31 with the through hole 33; the return spring is connected with the inner wall of the blind hole 36 and the ventilation block 32; a guide plate 34 which is flush with the upper end of the sliding chute 31 is arranged on the inner side wall of the sliding chute 31; when two adjacent strip-shaped sliding blocks 3 approach, the guide plate 34 enters the blind hole 36 to extrude the ventilation block 32, so that the ventilation block 32 moves to the through hole 33, the sliding groove 31 is in a closed state after the guide plate 34 enters the blind hole 36, and the concentrated sulfuric acid and the concentrated hydrochloric acid mixture in the sliding groove 31 are continuously pressed until the sliding groove 31 is communicated with the through hole 33 and then released. When in work, in the process of closing two adjacent strip-shaped sliding blocks 3, the guide plate 34 enters the blind hole 36 and pushes the ventilation block 32 to slide in the blind hole 36, so that the ventilation block 32 is communicated with the through hole 33 and the sliding groove 31 when reaching the through hole 33, when the guide plate 34 enters the blind hole 36 and the vent block 32 does not reach the through hole 33, the chute 31 is in a closed state, the mixture of concentrated sulfuric acid and concentrated hydrochloric acid in the chute 31 is pressed, after the vent block 32 is communicated with the through hole 33 and the chute 31, the concentrated sulfuric acid and the concentrated hydrochloric acid which are pressed in the chute 31 are extruded out instantly, thereby leading the concentrated sulfuric acid and the concentrated hydrochloric acid to be fully mixed to ensure that the concentrated hydrochloric acid is dehydrated and the hydrogen chloride in the concentrated hydrochloric acid overflows, leading the gasification rate of the hydrogen chloride in the concentrated hydrochloric acid to be improved, the hydrogen chloride is continuously dehydrated by the concentrated sulfuric acid which is leached from the upper part, so that the hydrogen chloride is dried, and high-quality hydrogen chloride gas with high purity and less moisture is obtained.
Further, two threads with opposite rotation directions are arranged on the surface of the power screw rod 41; the two sets of the mixing modules 2 are arranged, the mixing modules 2 on the upper portion of the hydrochloric acid guide pipe 14 and the mixing modules 2 on the lower portion of the hydrochloric acid guide pipe 14 are symmetrically arranged, the first sliding blocks 42 in the power module 4 are respectively located at two threads on the power screw rod 41, and the power screw rod 41 rotates to enable the two first sliding blocks 42 on the power screw rod 41 to slide away from or towards each other. The during operation, when the mixed module 2 of hydrochloric acid pipe 14 lower extreme is walked over to some concentrated sulfuric acid and concentrated hydrochloric acid mixture, the concentrated sulfuric acid is filled into in the spout 31 of bar slider 3 with the mixture of concentrated hydrochloric acid, draw close between the adjacent bar slider 3 and will extrude the concentrated sulfuric acid with the mixture of concentrated hydrochloric acid, make pressurized concentrated sulfuric acid and concentrated hydrochloric acid will be extruded away in the twinkling of an eye in the spout 31, thereby make the intensive mixing of concentrated sulfuric acid and concentrated hydrochloric acid and make the concentrated hydrochloric acid by the dehydration, hydrogen chloride in the concentrated hydrochloric acid spills over, the hydrogen chloride rate of gasification in the concentrated hydrochloric acid improves, and hydrogen chloride still can be continued the dehydration by the concentrated sulfuric acid that drenches from the top, make hydrogen chloride by the drying, thereby obtain the high-quality hydrogen chloride.
Further, a sleeve is fixedly arranged at the upper end of the through hole 33 on the strip-shaped sliding block 3; the upper end of the sleeve is rotatably connected with a cake block 35, and the sleeve is communicated with the through hole 33; a plurality of liquid outlet holes 351 are formed in the round cake block 35; and one end of each liquid outlet hole 351 is communicated with the sleeve, and the other end of each liquid outlet hole 351 is attached to the edge of the round cake block 35. The during operation, the back is given vent to anger from through-hole 33 to strong brine and concentrated sulfuric acid mixture in the spout 31, through the sleeve pipe get into in the cake piece 35 and along going out liquid hole 351 departure, because of going out liquid hole 351 the other end and the laminating of cake piece 35 edge, thereby make to drive cake piece 35 and rotate when strong brine and concentrated sulfuric acid spiral departure, be favorable to the intensive mixing of concentrated sulfuric acid and concentrated hydrochloric acid on the one hand, make the concentrated hydrochloric acid by the dehydration, on the other hand is favorable to the mixture separation of hydrogen chloride and concentrated hydrochloric acid and concentrated sulfuric acid, make the hydrogen chloride easily collected.
Further, an air outlet groove 43 is arranged at the air outlet 11; an air outlet block 44 is arranged at the air outlet groove 43; the edge of the gas outlet block 44 is provided with a gas outlet, the gas outlet block 44 falls on the gas outlet groove 43 under the action of self gravity to block the gas outlet 11, and the gas outlet block 44 is extruded by the hydrogen chloride gas to move upwards to communicate the gas outlet 11 with the gas outlet; an impeller 45 is arranged at the upper end of the power screw 41, and a coil spring 46 is arranged in the middle of the power screw 41; an air passage 47 is arranged above the air outlet block 44, and the air passage 47 is communicated with the impeller 45 in a tangential direction and then communicated with the outside of the reaction chamber 1; the impeller 45 rotates when the hydrogen chloride gas flows through, and the impeller 45 is reset and rotated by the coil spring 46 when the hydrogen chloride gas stops discharging. When the device works, after the pressure of hydrogen chloride gas in the reaction chamber 1 is increased, the hydrogen chloride gas can push the gas outlet block 44 to move upwards, the gas outlet hole is communicated with the reaction chamber 1 and the air passage 47 after the gas outlet block 44 moves upwards, and the hydrogen chloride gas impacts the impeller 45 to enable the power screw 41 to rotate, so that the power screw 41 has power without being driven by a motor, on one hand, the electric energy is saved, and on the other hand, the manufacturing cost of the device is reduced; and after the hydrogen chloride overflows from the gas outlet block 44, the pressure of the hydrogen chloride gas in the reaction chamber 1 is reduced, the gas outlet block 44 falls under the action of self gravity to block the gas outlet 11, so that the hydrogen chloride gas stops blowing to the impeller 45 for a short time, and the power screw 41 loses a power source for a short time, so that the power screw 41 is reversely rotated when the coil spring 46 is reset, two first sliders 42 on the power screw 41 return, two adjacent strip sliders 3 slide away, the power screw 41 is urged to rotate after the pressure of the hydrogen chloride gas in the reaction chamber 1 is increased for one time, and under the condition that concentrated hydrochloric acid and concentrated sulfuric acid are continuously introduced, the continuous preparation of the hydrogen chloride is realized.
Further, an elastic wiper blade 48 is arranged at the orifice of the blind hole 36; the upper end of the guide plate 34 is provided with an arc-shaped groove 49, and when the guide plate 34 enters the blind hole 36, the surface of the arc-shaped groove 49 on the guide plate 34 is scraped by the elastic scraper 48. During operation, concentrated sulfuric acid and concentrated sulfuric acid spray behind falling, partial concentrated sulfuric acid and concentrated hydrochloric acid mixture will spill on the arc recess 49 on the baffle 34, concentrated sulfuric acid and concentrated hydrochloric acid mixture is gathered on making the arc recess 49, at the in-process that baffle 34 got into blind hole 36, elastic doctor blade 48 on the blind hole 36 will gather concentrated sulfuric acid and concentrated hydrochloric acid mixture on the arc recess 49 and break away, thereby promote the abundant mixture of concentrated sulfuric acid and concentrated hydrochloric acid and make concentrated hydrochloric acid dehydrated, the hydrogen chloride in the concentrated hydrochloric acid spills over, make the hydrogen chloride gasification rate among the concentrated hydrochloric acid improve, and the hydrogen chloride still can be continued to dewater by the concentrated sulfuric acid that drenches from the top, make the hydrogen chloride dry, thereby obtain the high-quality hydrogen chloride gas that purity is high, the moisture is few.
The specific working process is as follows:
when the device works, concentrated sulfuric acid is downwards sprayed out from a sulfuric acid spray nozzle 13, the concentrated hydrochloric acid is sprayed out from a hydrochloric acid spray nozzle 15 after being guided in through a hydrochloric acid guide pipe 14, the concentrated sulfuric acid is mixed with the concentrated hydrochloric acid, the strong dehydration property of the concentrated sulfuric acid continuously extracts water in the hydrochloric acid and continuously releases heat, so that hydrogen chloride in the hydrochloric acid is absorbed and escaped, the hydrogen chloride gas is in countercurrent contact with the concentrated sulfuric acid continuously sprayed downwards when rising, the hydrogen chloride gas is fully dried, high-quality hydrogen chloride gas with high purity and less water is obtained from a gas outlet 11, and the dilute sulfuric acid is discharged from a discharge port 12; specifically, when the power screw 41 rotates forward and backward, the first sliding block 42 slides back and forth in the square cavity 16, the first sliding block 42 slides the suction sliding sleeve 21 back and forth on the hydrochloric acid conduit 14, and the first sliding block 42 slides the suction sliding sleeve 21 along with the suction sliding sleeve, so that the bar-shaped sliding blocks 3 hinged with the sliding sleeve 21 are pulled or pressed to cause the sliding between the adjacent bar-shaped sliding blocks 3; after concentrated sulfuric acid and concentrated hydrochloric acid are mixed and fall into the sliding groove 31 on the strip-shaped sliding block 3, the adjacent strip-shaped sliding blocks 3 slide to be close to each other, so that the two strip-shaped sliding blocks 3 jointly extrude a mixture of the concentrated sulfuric acid and the concentrated hydrochloric acid in the sliding groove 31, the concentrated sulfuric acid and the concentrated hydrochloric acid in the sliding groove 31 are blown to be mixed and dispersed under the sliding impact between the two adjacent strip-shaped sliding blocks 3, the concentrated sulfuric acid is effectively promoted to continuously extract water in the concentrated hydrochloric acid, heat is continuously released, hydrogen chloride in the hydrochloric acid is desorbed and escaped, overflowed hydrogen chloride is discharged from the gas outlet 11, and dry hydrogen chloride collection is realized;
after the pressure of the hydrogen chloride gas in the reaction chamber 1 is increased, the hydrogen chloride gas pushes the gas outlet block 44 to move upwards, the gas outlet hole is communicated with the reaction chamber 1 and the gas channel 47 after the gas outlet block 44 moves upwards, and the power screw 41 rotates due to the impact of the gas on the impeller 45, so that the power screw 41 has power without being driven by a motor, on one hand, the electric energy is saved, and on the other hand, the manufacturing cost of equipment is reduced; and after the hydrogen chloride overflows from the gas outlet block 44, the pressure of the hydrogen chloride gas in the reaction chamber 1 is reduced, the gas outlet block 44 falls under the action of self gravity to block the gas outlet 11, so that the hydrogen chloride gas stops blowing to the impeller 45 for a short time, and the power screw 41 loses a power source for a short time, so that the power screw 41 is reversely rotated when the coil spring 46 is reset, two first sliders 42 on the power screw 41 return, two adjacent strip sliders 3 slide away, the power screw 41 is urged to rotate after the pressure of the hydrogen chloride gas in the reaction chamber 1 is increased for one time, and under the condition that concentrated hydrochloric acid and concentrated sulfuric acid are continuously introduced, the continuous preparation of the hydrogen chloride is realized.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for preparing hydrogen chloride by a sulfuric acid extraction method is characterized by comprising the following steps: the method comprises the following steps:
s1, introducing concentrated hydrochloric acid into a hydrochloric acid conduit in the hydrogen chloride preparation device, introducing concentrated sulfuric acid into a sulfuric acid spray head in the hydrogen chloride preparation device, and preparing hydrogen chloride by using the hydrogen chloride preparation device;
s2, communicating the gas outlet of the hydrogen chloride preparation device in the S1 with two liquid storage tanks which are connected in series and are both filled with concentrated sulfuric acid, and sequentially filling hydrogen chloride into the two liquid storage tanks which are filled with concentrated sulfuric acid for drying;
s3, storing the collected hydrogen chloride gas in the storage tank for three to five minutes after the hydrogen chloride is prepared in S2;
s4, sleeving a sealing bag with a slaked lime layer on the storage tank of S3, and sealing the storage tank for collecting the hydrogen chloride by using the sealing bag;
the hydrogen chloride preparation devices in the S1 and S2 comprise a reaction chamber (1), a sulfuric acid spray nozzle (13) fixed on the upper part of the reaction chamber (1), a hydrochloric acid guide pipe (14) penetrating into the center of the lower end of the reaction chamber (1) from bottom to top, a hydrochloric acid spray nozzle (15), a mixing module (2) and a power module (4); the upper end of the reaction chamber (1) is provided with an air outlet (11) for collecting hydrogen chloride gas, one side of the lower end of the reaction chamber (1) is provided with a discharge port (12) for discharging dilute sulfuric acid, and the side wall of one side of the reaction chamber (1) is provided with a square cavity (16); the hydrochloric acid spray head (15) is arranged at the upper end of the hydrochloric acid guide pipe (14), and the hydrochloric acid spray head (15) is positioned at the lower end of the sulfuric acid spray head (13); the mixing module (2) comprises a sliding sleeve (21) and a stepped sliding extrusion strip; the sliding sleeve (21) is sleeved on the hydrochloric acid guide pipe (14), the sliding sleeve (21) is in sliding connection with the hydrochloric acid guide pipe (14), and the sliding sleeve (21) is a magnet; one end of each sliding extrusion strip is hinged with the sliding sleeve (21), the other end of each sliding extrusion strip is hinged with the side wall of the reaction chamber (1), and at least four sliding extrusion strips are arranged around the rotation center of the sliding sleeve (21); the sliding extrusion strip comprises a plurality of strip-shaped sliding blocks (3) and pull ropes; the strip-shaped sliding blocks (3) are provided with sliding grooves (31), adjacent strip-shaped sliding blocks (3) are connected in a sliding mode through the sliding grooves (31) and are arranged in a step shape, one strip-shaped sliding block (3) located at the end is hinged with the square sliding strip, and the other strip-shaped sliding block (3) located at the end is hinged with the side wall of the reaction chamber (1); the pull rope is used for connecting two adjacent strip-shaped sliding blocks (3) to avoid the sliding separation of the two adjacent strip-shaped sliding blocks (3); the power module (4) comprises a power lead screw (41) and a first sliding block (42); the power screw rod (41) and the first sliding block (42) are arranged at the square cavity (16) of the side wall of the reaction chamber (1); the first sliding block (42) is in sliding fit with the square cavity (16), and the first sliding block (42) is a magnet; the power screw rod (41) penetrates through the first sliding block (42), the power screw rod (41) rotates positively and negatively to drive the first sliding block (42) to slide back and forth in the square cavity (16) to attract the sliding sleeve (21) to slide along with the sliding, and the strip-shaped sliding blocks (3) hinged with the sliding sleeve (21) are pulled or pressed to cause the adjacent strip-shaped sliding blocks (3) to slide.
2. The method for preparing hydrogen chloride by the sulfuric acid extraction method as claimed in claim 1, wherein: a blind hole (36) is horizontally arranged at the upper part of one side of the strip-shaped sliding block (3); the blind hole (36) is internally provided with an air-through block (32) and a return spring, and the upper end of the middle part of the blind hole (36) is provided with a through hole (33) communicated with the outside of the strip-shaped sliding block (3); the ventilation block (32) is provided with a right-angle hole, and the ventilation block (32) slides to the through hole (33) in the blind hole (36) to communicate the inside of the sliding chute (31) with the through hole (33); the reset spring is connected with the inner wall of the blind hole (36) and the ventilation block (32); a guide plate (34) which is flush with the upper end of the sliding chute (31) is arranged on the inner side wall of the sliding chute (31); the guide plate (34) enters the blind hole (36) to extrude the ventilation block (32) when two adjacent strip-shaped sliding blocks (3) are close to each other, so that the ventilation block (32) moves to the through hole (33), the sliding groove (31) is in a closed state after the guide plate (34) enters the blind hole (36), and concentrated sulfuric acid and concentrated hydrochloric acid mixture in the sliding groove (31) is continuously pressed to the sliding groove (31) and is communicated with the through hole (33) and then released.
3. The method for preparing hydrogen chloride by the sulfuric acid extraction method as claimed in claim 2, wherein: the surface of the power screw rod (41) is provided with two threads with opposite rotation directions; the two sets of the mixing modules (2) are arranged, the mixing modules (2) on the upper portion of the hydrochloric acid guide pipe (14) and the mixing modules (2) on the lower portion of the hydrochloric acid guide pipe (14) are symmetrically arranged, the first sliding blocks (42) in the power module (4) are respectively located at two threads on the power lead screw (41), and the power lead screw (41) rotates to enable the first sliding blocks (42) on the power lead screw (41) to separate or slide in opposite directions.
4. The method for preparing hydrogen chloride by the sulfuric acid extraction method as claimed in claim 3, wherein: a sleeve is fixedly arranged at the upper end of the through hole (33) on the strip-shaped sliding block (3); the upper end of the sleeve is rotatably connected with a round cake block (35), and the sleeve is communicated with the through hole (33); a plurality of liquid outlet holes (351) are formed in the round cake block (35); and one ends of the liquid outlet holes (351) are communicated with the sleeve, and the other ends of the liquid outlet holes (351) are attached to the edge of the round cake block (35).
5. The method for preparing hydrogen chloride by the sulfuric acid extraction method as claimed in claim 3, wherein: an air outlet groove (43) is formed in the air outlet (11); an air outlet block (44) is arranged at the air outlet groove (43); the edge of the gas outlet block (44) is provided with a gas outlet hole, the gas outlet block (44) falls on the gas outlet groove (43) under the action of self gravity to block the gas outlet (11), and the gas outlet block (44) is extruded by the hydrogen chloride gas to move upwards to communicate the gas outlet (11) with the gas outlet hole; an impeller (45) is arranged at the upper end of the power screw rod (41), and a coil spring (46) is arranged in the middle of the power screw rod (41); an air passage (47) is arranged above the air outlet block (44), and the air passage (47) is communicated to the impeller (45) in a tangential direction and then communicated to the outside of the reaction chamber (1); the impeller (45) rotates when the hydrogen chloride gas flows through, and the impeller (45) is reset and rotated by the coil spring (46) when the hydrogen chloride gas stops discharging outwards.
6. The method for preparing hydrogen chloride by the sulfuric acid extraction method as claimed in claim 4, wherein: an elastic wiper blade (48) is arranged at the orifice of the blind hole (36); the upper end of the guide plate (34) is provided with an arc-shaped groove (49), and when the guide plate (34) enters the blind hole (36), the surface of the arc-shaped groove (49) on the guide plate (34) is scraped by the elastic scraper (48).
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| CN2161602Y (en) * | 1993-06-26 | 1994-04-13 | 苏州硫酸厂 | Hydrogen chloride generator by sulphuric acid extracting method |
| US6767528B2 (en) * | 1997-07-01 | 2004-07-27 | John E. Stauffer | Manufacture of hydrogen chloride from salt and sulfuric acid |
| CN1562732A (en) * | 2004-04-01 | 2005-01-12 | 上海交通大学 | Method for preparing strong hydrochloric acid through extracting and distilling deposed dilute hydrochloric acid semi continuously |
| CN102515105B (en) * | 2011-10-25 | 2013-10-09 | 山东农业大学 | Technological method for concentrating dilute hydrochloric acid through continuous extraction and rectification |
| CN108383085B (en) * | 2018-05-15 | 2023-05-26 | 杭州东日节能技术有限公司 | Device and method for preparing hydrogen chloride gas by full-resolution of hydrochloric acid by continuous method |
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Effective date of registration: 20201019 Address after: 239200 C area, industrial new district, Lai County, Anhui, Chuzhou Applicant after: CHUZHOU SANHE FIBER MANUFACTURING Co.,Ltd. Address before: 100089 Department of Mechanical and Electrical Engineering, Beijing University of Technology, No. 5 South Street, Zhongcun, Haidian District, Beijing Applicant before: Xie Zihao |
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