CN113387328A - Hydrogen chloride generator - Google Patents
Hydrogen chloride generator Download PDFInfo
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- CN113387328A CN113387328A CN202110908059.0A CN202110908059A CN113387328A CN 113387328 A CN113387328 A CN 113387328A CN 202110908059 A CN202110908059 A CN 202110908059A CN 113387328 A CN113387328 A CN 113387328A
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- hydrogen chloride
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- valve
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 177
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 title claims abstract description 177
- 229910000041 hydrogen chloride Inorganic materials 0.000 title claims abstract description 177
- 239000007789 gas Substances 0.000 claims abstract description 198
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 claims abstract description 22
- 238000009833 condensation Methods 0.000 claims description 29
- 230000005494 condensation Effects 0.000 claims description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 21
- 238000005057 refrigeration Methods 0.000 claims description 14
- 230000018044 dehydration Effects 0.000 claims description 12
- 238000006297 dehydration reaction Methods 0.000 claims description 12
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 11
- 239000001110 calcium chloride Substances 0.000 claims description 10
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 10
- 238000000746 purification Methods 0.000 claims description 9
- 230000005540 biological transmission Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 10
- 235000011148 calcium chloride Nutrition 0.000 description 9
- 230000001276 controlling effect Effects 0.000 description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 6
- 229940057995 liquid paraffin Drugs 0.000 description 6
- 238000007599 discharging Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 150000003841 chloride salts Chemical class 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 230000001174 ascending effect Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/03—Preparation from chlorides
- C01B7/035—Preparation of hydrogen chloride from chlorides
Abstract
The invention discloses a hydrogen chloride generator. Before collecting the hydrogen chloride gas, the gas cylinder is required to be filled with liquid, when the hydrogen chloride gas needs to be collected, the height of the level bottle is reduced through the lifting machine, the liquid in the gas cylinder flows into the level bottle, at the moment, the gas cylinder collects the hydrogen chloride produced by the hydrogen chloride generating unit until the gas cylinder is filled with the hydrogen chloride gas, then the level bottle is lifted, the liquid in the level bottle flows into the gas cylinder, and the hydrogen chloride gas in the gas cylinder is extruded and discharged to the gas production outlet pipeline.
Description
Technical Field
The invention relates to the field of gas preparation, in particular to a hydrogen chloride generator.
Background
Hydrogen chloride is an important raw material for synthesizing chlorohydrocarbon (chlorohydrocarbon can be obtained by reacting alcohol with hydrogen chloride), but hydrogen chloride gas with known, stable and controllable flow rate is difficult to obtain. Because hydrogen chloride gas is extremely corrosive, if a gas cylinder is used for supplying hydrogen chloride, special anti-corrosion treatment is required to be carried out on the gas cylinder, a valve and an instrument, and the cost is obviously increased. Even if antiseptic treatment is carried out, corrosion of hydrogen chloride gas to metal equipment such as gas cylinders, valves and instruments cannot be avoided, and serious safety risks can be caused by unpredictable leakage. Therefore, laboratories often utilize gas generators to provide hydrogen chloride gas for chemical reactions to avoid the potential safety hazard of storing highly corrosive hydrogen chloride gas. The chemical reaction in the hydrogen chloride gas generator is typically made by a metathesis reaction of concentrated sulfuric acid with a chloride salt, such as calcium chloride.
However, since the hydrogen chloride gas is supplied from the hydrogen chloride gas generator, the amount of hydrogen chloride generated is related to only the reaction rate, which is related to the amount of the reactant and the reaction temperature, which are both constantly changed as the reaction proceeds, so that the amount of hydrogen chloride gas generated becomes unstable and the flow rate becomes unknown.
Disclosure of Invention
In view of this, the embodiment of the present invention provides a hydrogen chloride generator to solve the problems of unstable gas amount and unknown flow rate of the hydrogen chloride produced in the prior art.
In order to achieve the above purpose, the embodiments of the present invention provide the following technical solutions:
a hydrogen chloride generator comprising: a hydrogen chloride generating unit, a hydrogen chloride purifying unit and a hydrogen chloride flow control unit;
the hydrogen chloride flow control unit comprises a level bottle, a gas measuring cylinder, a lifter and a comb-shaped pipe;
the first port of the comb-shaped pipe is communicated with the top of the gas measuring cylinder through a first valve;
the gas measuring cylinder is communicated with the level bottle and is used for collecting hydrogen chloride gas;
the second opening of the comb-shaped pipe is communicated with the hydrogen chloride generating unit through a second valve and the hydrogen chloride purifying unit;
the third opening of the comb-shaped pipe is communicated with a gas production outlet pipeline through a third valve;
the fourth opening of the comb-shaped pipe is connected with the outside through a fourth valve;
the lifter can drive the level bottle to move up and down, so that liquid flows back and forth between the level bottle and the air measuring cylinder.
Preferably, the bottom of the gas measuring cylinder is communicated with the bottom of the level bottle through a hose.
Preferably, the hydrogen chloride generation unit includes: a three-neck flask and a constant pressure dropping funnel;
a first opening of the three-opening flask is communicated with the hydrogen chloride purification unit, a second opening of the three-opening flask is communicated with the constant-pressure dropping funnel, and the three-opening flask is used for containing calcium chloride;
the constant-pressure dropping funnel is used for containing concentrated sulfuric acid.
Preferably, the three-neck flask further comprises a thermometer arranged at the third neck of the three-neck flask.
Preferably, the hydrogen chloride purification unit comprises: a water-removing bottle, a condensation bottle and a condenser;
the air inlet of the dehydration bottle is communicated with the air outlet of the hydrogen chloride generating unit, the air outlet is communicated with the air inlet of the condensation bottle, and concentrated sulfuric acid for dehydrating hydrogen chloride is contained in the dehydration bottle;
the air outlet of the condensation bottle is communicated with the second opening of the comb-shaped pipe;
the condenser is used for cooling the condensation bottle.
Preferably, the condenser includes: a low-temperature bath and a refrigeration temperature controller;
the condensation bottle is arranged in the low-temperature bath tank;
and the refrigeration temperature control instrument is used for controlling the refrigeration temperature of the refrigerating fluid in the low-temperature bath tank.
Preferably, the elevator comprises: the device comprises a motor, a controller, a lead screw and a tray;
the motor is in transmission connection with the lead screw, and the tray is arranged on the lead screw;
the controller is used for controlling the motor to drive the screw rod to rotate, so that the tray carries the level bottle to move up and down along the screw rod.
Preferably, the method further comprises the following steps: a three-way valve;
the gas inlet of the three-way valve is communicated with the gas outlet of the hydrogen chloride generating unit, the first gas outlet is communicated with the gas inlet of the hydrogen chloride purifying unit, and the second gas outlet is communicated with the first emptying pipeline.
Preferably, the method further comprises the following steps: a three-way switching valve;
an air inlet of the three-way switching valve is communicated with a first port of the comb-shaped pipe;
and a first air outlet of the three-way switching valve is communicated with a first emptying pipeline, and a second air outlet of the three-way switching valve is communicated with a gas production outlet pipeline.
Preferably, the method further comprises the following steps: and the gas buffer bottle is arranged between the gas inlet of the three-way switching valve and the first port of the comb-shaped pipe.
From the above, the invention discloses a hydrogen chloride generator, wherein the first port of the comb-shaped pipe is communicated with the top of the gas measuring cylinder through the first valve; the gas measuring cylinder is communicated with the leveling bottle, and the second opening of the comb-shaped pipe is communicated with the hydrogen chloride generating unit through a second valve and the hydrogen chloride purifying unit; a third port of the comb-shaped pipe is communicated with a gas production outlet pipeline through a third valve; connecting a fourth opening of the comb-shaped pipe with the outside through a fourth valve; before the hydrogen chloride gas is collected, the first valve and the fourth valve need to be opened, the second valve and the third valve need to be closed, then the elevator raises the level bottle, so that the liquid in the level bottle flows into the gas cylinder through the hose until the gas cylinder is filled with the liquid, when the hydrogen chloride gas needs to be collected, the first valve and the second valve need to be opened, the third valve and the fourth valve are closed, the height of the level bottle is lowered through the elevator, the liquid in the gas cylinder flows into the level bottle, at the moment, the gas cylinder collects the hydrogen chloride generated by the hydrogen chloride generating unit, after the gas cylinder is filled with the hydrogen chloride gas, the second valve and the fourth valve are closed, the first valve and the third valve are opened, then the level bottle is raised, so that the liquid in the level bottle flows into the gas cylinder, and the hydrogen chloride gas in the gas cylinder is extruded and discharged to the gas production outlet pipeline, in the application, because the gas cylinder is provided with scales, the discharge amount of the hydrogen chloride gas in unit time can be calculated by calculating the amount of the liquid flowing into the gas cylinder in unit time, and the discharge speed of the hydrogen chloride gas is controlled by adjusting the ascending speed of the elevator, so that the aims of controlling the hydrogen chloride output and stably outputting are fulfilled.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a hydrogen chloride generator according to an embodiment of the present invention.
The device comprises a 1-level bottle, a 2-three-neck flask, a 3-constant pressure dropping funnel, a 4-air measuring pipe, a 5-water removing bottle, a 6-condensation bottle, a 7-buffer bottle, an 8-three-way switching valve, a 9-three-way valve, a 10-first gas emptying pipeline, a 11-second gas emptying pipeline, a 12-gas production outlet pipeline, a 13-motor, a 14-controller, a 15-lead screw, a 16-lifter, a 17-comb-shaped pipe, an 18-thermometer, a 19-low temperature bath, a 20-refrigeration temperature controller, a 21-first valve, a 22-second valve, a 23-three valve and a 24-fourth valve.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In this application, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
An embodiment of the present invention provides a hydrogen chloride generator, and referring to fig. 1, fig. 1 is a schematic structural diagram of the hydrogen chloride generator, where the hydrogen chloride generator includes: a hydrogen chloride generating unit, a hydrogen chloride purifying unit and a hydrogen chloride flow control unit;
the hydrogen chloride flow control unit comprises a hydrogen chloride generating unit, a hydrogen chloride purifying unit and a hydrogen chloride flow control unit;
the hydrogen chloride flow control unit comprises a level bottle 1, a gas measuring cylinder 4, a lifter 16 and a comb-shaped pipe 17;
the first port of the comb-shaped pipe 17 is communicated with the top of the gas measuring cylinder 4 through a first valve 21;
the gas measuring cylinder 4 is communicated with the level bottle 1 and is used for collecting hydrogen chloride gas;
the second opening of the comb-shaped pipe 17 is communicated with the hydrogen chloride generating unit through a second valve 22;
a third port of the comb-shaped pipe 17 is communicated with the gas production outlet pipeline 12 through a third valve 23;
the fourth port of the comb-shaped pipe 17 is connected with the outside through a fourth valve 24;
the lifter 16 can move the level vial 1 up and down, so that the liquid flows back and forth between the level vial 1 and the gas measuring cylinder 4.
It should be noted that the gas measuring cylinder 4 is a graduated cylinder, and the first port of the comb-shaped pipe 17 is communicated with the top of the gas measuring cylinder 4 through a first valve 21; the gas measuring cylinder 4 is communicated with the level bottle 1, and the second opening of the comb-shaped pipe 17 is communicated with the hydrogen chloride generating unit through a second valve 22 and the hydrogen chloride purifying unit; a third port of the comb-shaped pipe 17 is communicated with the gas production outlet pipeline 12 through a third valve 23; and the fourth port of the comb-shaped pipe 17 is connected with the outside through a fourth valve 24; before collecting the hydrogen chloride gas, the first valve 21 and the fourth valve 24 are opened, the second valve 22 and the third valve 23 are closed, then the elevator 16 raises the level bottle 1 to make the liquid in the level bottle 1 flow into the gas cylinder 4 through the hose until the gas cylinder 4 is filled with the liquid, when the hydrogen chloride gas needs to be collected, the first valve 21 and the second valve 22 are opened, the third valve 23 and the fourth valve 24 are closed, the elevator 16 lowers the height of the level bottle 1 to make the liquid in the gas cylinder 4 flow into the level bottle 1, at this time, the gas cylinder 4 collects the hydrogen chloride generated by the hydrogen chloride generating unit, after the gas cylinder 4 is filled with the hydrogen chloride gas, the second valve 22 and the fourth valve 24 are closed, the first valve 21 and the third valve 23 are opened, then the level bottle 1 is raised to make the liquid in the level bottle 1 flow into the gas cylinder 4, the hydrogen chloride gas in the gas measuring cylinder 4 is extruded and discharged to the gas production outlet pipeline 12, in the application, the gas measuring cylinder 4 is provided with scales, so that the discharge amount of the hydrogen chloride gas in unit time can be calculated by calculating the amount of liquid flowing into the gas measuring cylinder 4 in unit time, the discharge speed of the hydrogen chloride gas is controlled by adjusting the ascending speed of the elevator, and the purposes of controlling the hydrogen chloride output and stably outputting are achieved.
Since the liquid is liquid sodium rock, which does not chemically react with hydrogen chloride, the amount of hydrogen chloride produced can be calculated by calculating the amount of liquid sodium rock per unit inflow amount of the gas cylinder 4 when hydrogen chloride gas is discharged from the gas cylinder 4.
Specifically, the bottom of the gas measuring cylinder 4 is communicated with the bottom of the level bottle 1 through a hose.
It should be noted that the bottom of the gas measuring cylinder 4 is communicated with the bottom of the level bottle 1 through a hose, so that when collecting hydrogen chloride gas, the level bottle 1 can be lowered through the lifter 16, and further, the liquid in the gas measuring cylinder 4 can be conveniently and completely discharged to the level bottle 1, so that more hydrogen chloride gas can be collected in the gas measuring cylinder 4, and the hydrogen chloride collecting efficiency is effectively improved.
When the gas cylinder 4 and the level vial 1 are connected to each other by a hose, one end of the hose is connected to the middle position of the gas cylinder 4, and the other end of the hose is connected to the bottom of the level vial 1, and when the hydrogen chloride gas is to be collected, the level vial 1 is lowered by the lifter 16, so that the liquid in the gas cylinder 4 at a position higher than the hose connection position flows back to the level vial 1, and then the gas cylinder 4 collects the hydrogen chloride gas.
Specifically, the hydrogen chloride generation unit includes: a three-neck flask 2 and a constant pressure dropping funnel 3;
a first opening of the three-mouth flask 2 is communicated with a hydrogen chloride purification unit, a second opening of the three-mouth flask 2 is communicated with a constant pressure dropping funnel 3, and the three-mouth flask 2 is used for containing calcium chloride;
the constant pressure dropping funnel 3 is used for containing concentrated sulfuric acid.
It should be noted that the first opening of the three-mouth flask 2 is communicated with the hydrogen chloride purification unit, the second opening is communicated with the constant pressure dropping funnel 3, calcium chloride is contained in the three-mouth flask 2, the constant pressure dropping funnel 3 contains concentrated sulfuric acid, and when the hydrogen chloride gas is collected, only the constant pressure dropping funnel 3 needs to contain the concentrated sulfuric acid to drop into the three-mouth flask 2, so that the calcium chloride is contacted with the concentrated sulfuric acid and a chemical reaction is carried out to generate the hydrogen chloride gas.
It should also be noted that the three-neck flask 2 may contain calcium chloride, and may also contain other chloride salts, such as magnesium chloride.
Further, the hydrogen chloride generator also comprises a thermometer 18 arranged at the third opening of the three-opening flask 2.
It should be noted that, by arranging the thermometer at the third port of the three-necked flask 2, the temperature in the three-necked flask 2 can be monitored in real time through the thermometer 18, so that damage to the three-necked flask 2 caused by overhigh temperature in the three-necked flask 2 is avoided, and the personal safety of experimenters is effectively ensured.
Specifically, the hydrogen chloride purification unit includes: a water-removing bottle 5, a condensing bottle 6 and a condenser;
an air inlet of the dehydration bottle 5 is communicated with an air outlet of the hydrogen chloride generation unit, the air outlet is communicated with an air inlet of the condensation bottle 6, and concentrated sulfuric acid for dehydrating the hydrogen chloride is contained in the dehydration bottle 5;
the air outlet of the condensation bottle 6 is communicated with the second opening of the comb-shaped pipe 17;
the condenser is used for cooling the condensation bottle 6.
It should be noted that concentrated sulfuric acid for dehydrating hydrogen chloride is contained in the dehydration bottle 5, an air inlet of the dehydration bottle 5 is connected with an air outlet of the hydrogen chloride generation unit, the air outlet is communicated with an air inlet of the condensation bottle 6, the air outlet of the condensation bottle 6 is communicated with the second opening of the comb-shaped pipe 17, the condensation bottle 6 is cooled through the condenser, hydrogen chloride produced from the hydrogen chloride generation unit is dehydrated through the concentrated sulfuric acid in the dehydration bottle 5, and then is condensed through the condensation bottle 6, so that low-temperature dried hydrogen chloride gas can be obtained, and the purity of the hydrogen chloride gas is effectively improved.
Further, the condenser includes: a low-temperature bath 19 and a refrigeration temperature controller 20;
the condensation bottle 6 is arranged in the low-temperature bath 19;
the refrigeration temperature controller 20 is used for controlling the refrigeration temperature of the refrigerant liquid in the low-temperature bath 19.
The condensation flask 6 is disposed in the low-temperature bath 19; and the refrigeration temperature control instrument 20 is used for controlling the refrigeration temperature of the refrigerating fluid in the low-temperature bath 19, so that the temperature of the condensation bottle 6 is in a preset temperature range, namely-5 degrees to-15 degrees, and the over-low or over-high temperature of the condensation bottle 6 is avoided to influence the hydrogen chloride gas production efficiency.
Specifically, the elevator includes: a motor 13, a controller 14, a lead screw 15 and a tray;
the motor 13 is in transmission connection with the lead screw 15, and the tray is arranged on the lead screw 15;
the controller 14 is used for controlling the motor to drive the screw rod 15 to rotate, so that the tray carries the level bottle 1 to move up and down along the screw rod 15.
It should be noted that the motor 13 is in transmission connection with the lead screw 15, the tray is arranged on the lead screw 15, and the controller 14 controls the motor to drive the lead screw 15 to rotate, so that the tray carries the level bottle 1 to move up and down along the lead screw 15, and further, the liquid flows back and forth between the level bottle 1 and the gas measuring cylinder 4, and the purposes of collecting hydrogen chloride and discharging hydrogen chloride gas are achieved.
The controller 14 is a variable frequency controller, and can control the rotation speed of the motor 13, and thus the lifting speed of the level vial 1 carried on the pallet.
It is noted that the lifting mechanism of the present application is composed of the motor 13, the controller 14, the lead screw 15 and the tray, but the lifting mechanism may also be composed of other components for driving the level vial 1 to lift, and therefore, the lifting mechanism is not limited to be composed of the motor 13, the controller 14, the lead screw 15 and the tray.
Further, the hydrogen chloride generator also includes: a three-way valve 9;
the air inlet of the three-way valve 9 is communicated with the air outlet of the hydrogen chloride generating unit, the first air outlet is communicated with the air inlet of the hydrogen chloride purifying unit, and the second air outlet is communicated with the first emptying pipeline 10.
It should be noted that, by setting up the three-way valve 9, and communicate the air inlet of the three-way valve 9 with the air outlet of the hydrogen chloride generating unit, first air outlet communicates with the air inlet of the hydrogen chloride purifying unit, the second air outlet communicates with the first emptying pipeline 10, before the hydrogen chloride is collected for the first time, because there are various impurity gases in the device, therefore, the first air outlet of the three-way valve 9 needs to be closed, the second air outlet is opened, when the hydrogen chloride generating unit produces hydrogen chloride, the produced hydrogen chloride and impurities can be discharged together through the first emptying pipeline 10, and after the impurities in the hydrogen chloride generating unit are discharged, the second outlet is closed, the first outlet is opened, the hydrogen chloride produced by the hydrogen chloride generating unit enters the hydrogen chloride purifying unit and the hydrogen chloride flow control unit to be collected, so as to ensure the purity of the hydrogen chloride gas.
Further, the hydrogen chloride generator also includes: a three-way switching valve 8;
the air inlet of the three-way switching valve 8 is communicated with the first port of the comb-shaped pipe 17;
a first air outlet of the three-way switching valve 8 is communicated with a first emptying pipeline 11, and a second air outlet is communicated with a gas production outlet pipeline 12.
It should be noted that, by providing the three-way switching valve 8, the air inlet of the three-way switching valve 8 is communicated with the first port of the comb-shaped pipe 17; the first gas outlet of the three-way switching valve 8 is communicated with a first emptying pipeline 11, the second gas outlet of the three-way switching valve 8 is communicated with a gas production outlet pipeline 12, other gases in the pipeline between the three-way switching valve 8 and the comb-shaped pipe 17 can be discharged by closing the second gas outlet of the three-way switching valve 8 and opening the first gas outlet of the three-way switching valve 8, the influence of the gas in the pipeline on the purity of the hydrogen chloride gas is avoided, and after other gases in the pipeline are emptied, the second gas outlet of the three-way switching valve 8 is opened and the first gas outlet of the three-way switching valve 8 is closed, so that the produced hydrogen chloride gas is conveyed to the gas production outlet pipeline 12.
Further, the hydrogen chloride generator also includes: and the gas buffer bottle 7 is arranged between the gas inlet of the three-way switching valve 8 and the first port of the comb-shaped pipe 17.
By providing the gas buffer bottle 7, the fine powder in the hydrogen chloride gas can be purified, and the hydrogen chloride gas can be purified to a higher purity.
To facilitate understanding of the above solution, the solution is further described below with reference to fig. 1.
A hydrogen chloride generating and stable output device comprises a hydrogen chloride generating unit, a hydrogen chloride purifying unit and a hydrogen chloride flow control unit.
The hydrogen chloride generating unit comprises a three-neck flask 2, concentrated sulfuric acid, chloride and a constant pressure dropping funnel 3.
Preferably, the chloride salt is calcium chloride or magnesium chloride.
Preferably, the middle port of the three ports of the three-mouth flask 2 is connected with the constant pressure dropping funnel 3, and the two ports are respectively connected with the gas outlet and the thermometer 18.
The hydrogen chloride purification unit consists of a water removal bottle 5 and a condensation bottle 6.
Preferably, concentrated sulfuric acid with the concentration of 95-98% or anhydrous calcium chloride particles are contained in the dehydration bottle 5.
Preferably, the condensation bottle 6 is a glass empty bottle, and is placed in the low-temperature bath 19, and the refrigeration liquid in the low-temperature bath 19 is refrigerated and temperature-controlled by the refrigeration temperature controller 20.
Preferably, the temperature of the condensation bottle 6 is-5 to-15 ℃.
The hydrogen chloride flow control unit consists of a level bottle 1, a gas measuring pipe 4, a constant-speed lifter 16, a comb-shaped pipe 17, a buffer bottle 7, a tee joint 9, a three-way switching valve 8 and four two-way valves positioned on the comb-shaped pipe 17, namely a first valve 21, a second valve 22, a third valve 23 and a fourth valve 24, wherein a gas outlet of the three-mouth flask 2 is connected with one inlet of the tee joint 9, two outlets of the tee joint 9 are respectively connected with an emptying pipeline 10 and a dehydration bottle 5, the bottom of the gas measuring pipe 4 is connected with the level bottle 1 through a hose, an outlet at the top of the gas measuring pipe 4 is respectively connected with a gas buffer bottle 6 and the gas buffer bottle 7, an outlet of the gas buffer bottle 7 is connected with the three-way switching valve 8, and two outlets of the three-way switching valve 8 are respectively connected with the emptying pipeline 11 or a gas production outlet pipeline 12.
Preferably, the gas measuring tube 4 is a graduated glass tube.
Preferably, the buffer bottle 7 is an empty glass bottle.
Preferably, the level vial 1 contains liquid paraffin.
Preferably, the uniform-speed lifter 16 is composed of a variable-frequency motor 13, a variable-frequency controller 14 and a lead screw 15, and the lifting speed can be regulated and controlled by the variable-frequency controller 14.
Preferably, the four two-way valves and the pipes on the comb-shaped pipe 17 are made of glass or polytetrafluoroethylene.
The method comprises the following operation steps: step one, opening a first valve 21 and a fourth valve 24, closing a second valve 22 and a third valve 23, and filling part of liquid paraffin in the level bottle 1 into the air measuring pipe 4 by increasing the liquid level of the level bottle 1.
And step two, after the gas measuring pipe 4 is filled with the liquid paraffin, closing the first valve 21 and the fourth valve 24, and sealing the liquid paraffin in the gas measuring pipe 4.
And step three, dropwise adding concentrated sulfuric acid onto chloride in the three-neck flask 2 through the constant-pressure dropping funnel 3, carrying out double decomposition reaction on the concentrated sulfuric acid and the chloride to generate hydrogen chloride gas, and enabling the hydrogen chloride gas to enter the connected emptying pipeline 10 after passing through the three-way valve 9.
And step four, after the original gas in the upstream pipeline of the three-way valve 9 and the three-neck flask 2 is fully replaced by the hydrogen chloride, opening the first valve 21 and the second valve 22, reducing the height of the leveling bottle, correspondingly reducing the liquid level of the liquid paraffin in the gas measuring pipe 4, and sucking the hydrogen chloride gas into the gas measuring pipe 4 through the degassing bottle 5 and the condensation bottle 6.
Step five, after the gas measuring pipe 4 is filled with the hydrogen chloride gas, closing the first valve 21 and the second valve 22 of the valves, opening the third valve 23, placing the three-way switching valve 8 in the emptying direction, lifting the height of the level bottle 1, enabling the liquid paraffin to enter the gas measuring pipe 4, and enabling the hydrogen chloride gas in the gas measuring pipe 4 to flow through the gas buffer bottle 7 and the emptying pipeline 11 of the three-way switching valve 8 and then be emptied.
And step six, after the hydrogen chloride gas in the gas measuring pipe 4 is completely emptied, closing the third valve 23, opening the first valve 21 and the second valve 22, sucking the hydrogen chloride gas into the gas measuring pipe 4 by the same flow, opening the third valve 23, closing the first valve 21 and the second valve 22, discharging the hydrogen chloride gas out of the gas measuring pipe 4 by the same flow, and fully replacing the original gas in the downstream pipeline of the gas measuring pipe 4 and the buffer bottle 7 with the hydrogen chloride gas after repeating for multiple times.
And seventhly, the three-way switching valve 8 is turned to a gas production outlet pipeline 12, the leveling bottle 1 is lifted at a constant speed along a screw rod 15 through a constant speed lifter 16, hydrogen chloride gas in the gas measuring pipe 4 is discharged at a constant speed, the lifting speed of the lifter can be regulated and controlled through a variable frequency controller 14, and HCl gas with known flow is stably output through the gas production outlet pipeline 12.
Example 1: weighing 350g of CaCl2, putting into a three-neck flask, and putting 250ml of concentrated sulfuric acid into a constant-pressure dropping funnel; dropwise adding concentrated sulfuric acid into a three-neck flask, and starting HCl gas production reaction; 95-98% concentrated sulfuric acid is filled in the dehydration bottle, and the temperature of the condensation bottle is-15 ℃; setting the gas outlet of the three-way switching valve in a gas emptying pipeline, and fully replacing the original gas in the pipeline with hydrogen chloride gas by repeatedly sucking and discharging HCl gas; after replacement, the three-way switching valve is switched to the HCl gas production output pipeline, the level bottle is lifted at a constant speed through the lifter, hydrogen chloride gas in the gas measuring pipe is discharged at a constant speed, the working frequency of the frequency conversion controller of the lifter is 10Hz, and the gas outlet flow is 2 ml/min.
Example 2: the same operation procedure as in example 1 was adopted, the temperature of the condensation flask was-10 deg.C, the operating frequency of the frequency-variable controller of the elevator was 30Hz, and the outlet gas flow rate was 6 ml/min.
Example 3: 350g of MgCl2 is weighed and put into a three-neck flask, and 250ml of concentrated sulfuric acid is put into a constant pressure dropping funnel; dropwise adding concentrated sulfuric acid into a three-neck flask, and starting HCl gas production reaction; calcium chloride particles are filled in the dehydration bottle, and the temperature of the condensation bottle is-5 ℃; setting the gas outlet of the three-way switching valve in a gas emptying pipeline, and fully replacing the original gas in the pipeline with hydrogen chloride gas by repeatedly sucking and discharging HCl gas; after replacement, the three-way switching valve is switched to the HCl gas production output pipeline, the level bottle is lifted at a constant speed through the lifter, hydrogen chloride gas in the gas measuring pipe is discharged at a constant speed, the working frequency of the frequency conversion controller of the lifter is 20Hz, and the gas outlet flow is 4 ml/min.
Example 4: the same operation procedure as in example 3 was adopted, the temperature of the condensation flask was-10 deg.C, the operating frequency of the frequency-variable controller of the elevator was 40Hz, and the outlet flow rate was 8 ml/min.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, the system or system embodiments are substantially similar to the method embodiments and therefore are described in a relatively simple manner, and reference may be made to some of the descriptions of the method embodiments for related points. The above-described system and system embodiments are merely illustrative, wherein units described as separate components may or may not be physically separate, and components shown as units may or may not be physical units, may be located in one place, or may be distributed on a plurality of network units. Some or all of the modules may be selected according to actual needs to achieve the purpose of the solution of the present embodiment. One of ordinary skill in the art can understand and implement it without inventive effort.
Those of skill would further appreciate that the various illustrative elements and algorithm steps described in connection with the embodiments disclosed herein may be implemented as electronic hardware, computer software, or combinations of both, and that the various illustrative components and steps have been described above generally in terms of their functionality in order to clearly illustrate this interchangeability of hardware and software. Whether such functionality is implemented as hardware or software depends upon the particular application and design constraints imposed on the implementation. Skilled artisans may implement the described functionality in varying ways for each particular application, but such implementation decisions should not be interpreted as causing a departure from the scope of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A hydrogen chloride generator, comprising: a hydrogen chloride generating unit, a hydrogen chloride purifying unit and a hydrogen chloride flow control unit;
the hydrogen chloride flow control unit comprises a level bottle (1), a gas measuring cylinder (4), a lifter (16) and a comb-shaped pipe (17);
the first opening of the comb-shaped pipe (17) is communicated with the top of the air measuring cylinder (4) through a first valve (21);
the gas measuring cylinder (4) is communicated with the level bottle (1) and is used for collecting hydrogen chloride gas;
a second opening of the comb-shaped pipe (17) is communicated with the hydrogen chloride purification unit and the hydrogen chloride generation unit through a second valve (22);
a third opening of the comb-shaped pipe (17) is communicated with a gas production outlet pipeline (12) through a third valve (23);
a fourth opening of the comb-shaped pipe (17) is connected with the outside through a fourth valve (24);
the lifter (16) can drive the level bottle (1) to move up and down, so that liquid flows back and forth between the level bottle (1) and the air measuring cylinder (4).
2. The hydrogen chloride generator according to claim 1, characterized in that the bottom of the gas measuring cylinder (4) communicates with the bottom of the level vial (1) through a hose.
3. The hydrogen chloride generator according to claim 1, wherein the hydrogen chloride generating unit comprises: a three-neck flask (2) and a constant pressure dropping funnel (3);
a first opening of the three-mouth flask (2) is communicated with the hydrogen chloride purification unit, a second opening of the three-mouth flask is communicated with the constant-pressure dropping funnel (3), and the three-mouth flask (2) is used for containing calcium chloride;
the constant-pressure dropping funnel (3) is used for containing concentrated sulfuric acid.
4. The hydrogen chloride generator according to claim 3, further comprising a thermometer (18) provided to a third port of the three-necked flask (2).
5. The hydrogen chloride generator according to claim 1, wherein the hydrogen chloride purification unit comprises: a water-removing bottle (5), a condensing bottle (6) and a condenser;
the air inlet of the water removal bottle (5) is communicated with the air outlet of the hydrogen chloride generating unit, the air outlet is communicated with the air inlet of the condensation bottle (6), and concentrated sulfuric acid for hydrogen chloride dehydration is contained in the water removal bottle (5);
the air outlet of the condensation bottle (6) is communicated with the second opening of the comb-shaped pipe (17);
the condenser is used for cooling the condensation bottle (6).
6. The hydrogen chloride generator of claim 5, wherein the condenser comprises: a low-temperature bath (19) and a refrigeration temperature controller (20);
the condensation bottle (6) is arranged in the low-temperature bath (19);
the refrigeration temperature control instrument (20) is used for controlling the refrigeration temperature of the refrigerating fluid in the low-temperature bath (19).
7. The hydrogen chloride generator of claim 1, wherein the elevator comprises: the device comprises a motor (13), a controller (14), a lead screw (15) and a tray;
the motor (13) is in transmission connection with the lead screw (15), and the tray is arranged on the lead screw (15);
the controller (14) is used for controlling the motor to drive the screw rod (15) to rotate, so that the tray carries the level bottle (1) to move up and down along the screw rod (15).
8. The hydrogen chloride generator of claim 1, further comprising: a three-way valve (9);
the air inlet of the three-way valve (9) is communicated with the air outlet of the hydrogen chloride generating unit, the first air outlet is communicated with the air inlet of the hydrogen chloride purifying unit, and the second air outlet is communicated with the first emptying pipeline (10).
9. The hydrogen chloride generator of claim 1, further comprising: a three-way switching valve (8);
an air inlet of the three-way switching valve (8) is communicated with a first port of the comb-shaped pipe (17);
and a first air outlet of the three-way switching valve (8) is communicated with a first emptying pipeline (11), and a second air outlet is communicated with a gas production outlet pipeline (12).
10. The hydrogen chloride generator of claim 9, further comprising: and the gas buffer bottle (7) is arranged between the gas inlet of the three-way switching valve (8) and the first port of the comb-shaped pipe (17).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115979777A (en) * | 2023-03-20 | 2023-04-18 | 苏州冠德能源科技有限公司 | Infrared spectrum-based preparation system, method and detection method for chlorine isotope sample in chlorohydrocarbon |
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Application publication date: 20210914 |