CN112206729A - Method for recovering aluminum chloride by aiming at crude zirconium tetrachloride purification seeds - Google Patents
Method for recovering aluminum chloride by aiming at crude zirconium tetrachloride purification seeds Download PDFInfo
- Publication number
- CN112206729A CN112206729A CN202010991513.9A CN202010991513A CN112206729A CN 112206729 A CN112206729 A CN 112206729A CN 202010991513 A CN202010991513 A CN 202010991513A CN 112206729 A CN112206729 A CN 112206729A
- Authority
- CN
- China
- Prior art keywords
- block
- aluminum chloride
- zirconium tetrachloride
- fixedly connected
- filter plate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- VSCWAEJMTAWNJL-UHFFFAOYSA-K Aluminium chloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 title claims abstract description 106
- DUNKXUFBGCUVQW-UHFFFAOYSA-J Zirconium(IV) chloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 title claims abstract description 61
- 238000000746 purification Methods 0.000 title claims abstract description 27
- VZGDMQKNWNREIO-UHFFFAOYSA-N Carbon tetrachloride Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims abstract description 64
- 229910052751 metal Inorganic materials 0.000 claims abstract description 23
- 239000002184 metal Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 230000001376 precipitating Effects 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 2
- 238000000859 sublimation Methods 0.000 abstract description 2
- 230000002277 temperature effect Effects 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 11
- 230000000694 effects Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 230000000630 rising Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- -1 aluminum chloride Chemical compound 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Other filters with filtering elements stationary during filtration, e.g. pressure or suction filters, or filtering elements therefor
- B01D29/01—Other filters with filtering elements stationary during filtration, e.g. pressure or suction filters, or filtering elements therefor with flat filtering elements
- B01D29/03—Other filters with filtering elements stationary during filtration, e.g. pressure or suction filters, or filtering elements therefor with flat filtering elements self-supporting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Other filters with filtering elements stationary during filtration, e.g. pressure or suction filters, or filtering elements therefor
- B01D29/50—Other filters with filtering elements stationary during filtration, e.g. pressure or suction filters, or filtering elements therefor with multiple filtering elements, characterised by their mutual disposition
- B01D29/56—Other filters with filtering elements stationary during filtration, e.g. pressure or suction filters, or filtering elements therefor with multiple filtering elements, characterised by their mutual disposition in series connection
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
- C01F7/62—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/04—Halides
Abstract
The invention provides a method for recovering aluminum chloride from crude zirconium tetrachloride purification seeds, and provides a device for recovering aluminum chloride from crude zirconium tetrachloride purification seeds. This aluminium chloride device is retrieved to thick zirconium tetrachloride purification seed, through the inside temperature of thermistor control reaction chamber, thermistor and electromagnetic means electric connection, electromagnetic means is driving the second metal ball through the third magnetic path and is sliding on the variable resistance, thereby change the resistance value of variable resistance, the power of heater in the control reaction chamber, thereby prevent that the high temperature from leading to the aluminium chloride sublimation or the low carbon tetrachloride that leads to of temperature can not volatilize, thereby reached automatic control temperature's effect.
Description
Technical Field
The invention relates to the technical field of purification of crude zirconium tetrachloride, in particular to a method for recovering aluminum chloride from a crude zirconium tetrachloride purification seed.
Background
Zirconium tetrachloride is white crystal powder at normal temperature, is mainly and intensively applied to material science or used as a catalyst, and often generates a plurality of impurities in industrial purification of crude zirconium tetrachloride, such as aluminum chloride, which not only can be used as an organic chemical catalyst, but also can be used for metal smelting and the like, and belongs to one of important materials in industrial manufacture.
At present, the device for recovering aluminum chloride in the purification of crude zirconium tetrachloride is imperfect, aluminum chloride in the crude zirconium tetrachloride cannot be fully separated, resource waste is caused, meanwhile, the existing industry adopts manual operation to operate, not only can labor burden be brought to workers, but also the working efficiency is low, and therefore the device for recovering aluminum chloride in the purification of crude zirconium tetrachloride is provided for solving the problems.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for recovering aluminum chloride from a crude zirconium tetrachloride purification seed, which is achieved by the following specific technical means:
a method for recovering aluminum chloride from crude zirconium tetrachloride purification seeds comprises the following steps:
s1, firstly, introducing crude zirconium tetrachloride containing aluminum chloride impurities into a carbon tetrachloride solution, dissolving aluminum chloride in carbon tetrachloride by stirring, controlling the rotating speed to operate at 30 revolutions per minute, and precipitating the zirconium tetrachloride at the bottom of the carbon tetrachloride solution;
s2, evaporating the carbon tetrachloride solution on the surface of the zirconium tetrachloride when the temperature of the left end outlet of the heating furnace is between 78 and 170 ℃, and discharging the zirconium tetrachloride out of the furnace in an extraction mode;
s3; and finally, heating the indoor temperature to 90-170 ℃ by utilizing the difference of the boiling points of the carbon tetrachloride and the aluminum chloride, volatilizing the carbon tetrachloride indoors, and heating the aluminum chloride into white particles to precipitate on the indoor bottom end.
The method for recovering aluminum chloride from crude zirconium tetrachloride purification seeds as claimed in claim 1, further comprising a casing rotatably connected with a drive shaft in the middle, wherein a first long rod is rotatably connected to the lower end of the drive shaft, a second long rod is arranged at the bottom end of the first long rod, feed pipes are arranged on two sides of the casing, a switch device is arranged at the bottom end of each feed pipe, a first notch is formed in the switch device, a first push block is slidably connected in the casing, a metal block is fixedly connected in the first push block, an air bag is fixedly connected at the bottom end of the first push block, a first metal ball is arranged at the lower end of the air bag, a second push block is arranged in the casing and at the end of the first notch far from the first push block, and a first stop block is arranged at the end of the second push block far from the first push block, the surface of the first stop block is provided with a second notch, the bottom end of the second long rod is provided with a first filter plate, two ends of the first filter plate are fixedly connected with a rotating block, the inside of the rotating block is slidably connected with a third push block, the inside of the third push block is slidably connected with a clamping block, the bottom end of the first filter plate is provided with a second filter plate, the left side of the second filter plate is provided with a pipe drawing, the right side of the second filter plate is provided with a reaction chamber, the inside of the reaction chamber is fixedly connected with a heating wire, the upper end of the heating wire is provided with a collecting plate, the left side of the collecting plate is fixedly connected with a first magnetic block, the upper part of the first magnetic block is provided with a second magnetic block, the surface of the second magnetic block is fixedly connected with a second stop block, two sides of the reaction chamber are fixedly, the electromagnetic device is characterized in that a third magnetic block is arranged on the right side of the electromagnetic device, a second metal ball is fixedly connected to the surface of the third magnetic block, the second metal ball is connected with a variable resistor in a sliding mode, a water tank is arranged on the right side of the control device, a cooling device is arranged on the upper portion of the water tank, and a collecting pipe is arranged on the right side of the water tank.
Preferably, the second push block is connected in the first notch in a sliding manner, and the air bag drives the first push block to slide in the first notch by the rising of the liquid level to extrude the air in the first notch, so that the second push block slides in the first notch.
Preferably, a clamping block fixedly connected to the surface of the third pushing block is matched with a second notch formed in the surface of the first stopping block, the third pushing block is pushed by the second pushing block, the clamping block is separated from the second notch, and the rotating block drives the first filter plate to rotate.
Preferably, the second filter sets up in the inside slope of casing for zirconium tetrachloride slides the speed on the second filter, and carbon tetrachloride and aluminium chloride mixed liquid have the pushing action to zirconium tetrachloride simultaneously.
Preferably, the thermistor is electrically connected with the electromagnetic device, a magnetic pole of a magnetic field generated by the electromagnetic device is the same as a magnetic pole of a third magnetic block opposite to the magnetic pole, and the electromagnetic device drives the second metal ball to slide on the variable resistor through the third magnetic block.
Preferably, the magnetic pole of the first magnetic block is opposite to that of the second magnetic block opposite to the magnetic pole of the second magnetic block, the second magnetic block is fixed inside the second stop block, and the collecting plate can control the second stop block to slide up and down in the reaction chamber through the first magnetic block.
Advantageous effects
Compared with the prior art, the invention provides a method for recovering aluminum chloride from crude zirconium tetrachloride purification seeds, which has the following beneficial effects:
1. the method for recovering aluminum chloride by aiming at the purification of crude zirconium tetrachloride comprises the steps that when the zirconium tetrachloride on the surface of a first filter plate is excessive, the zirconium tetrachloride can block filter holes of the first filter plate to cause the liquid level of carbon tetrachloride in a shell to rise, the rising liquid level drives a first push block to move upwards by pushing an air bag in a first notch, the first push block pushes air in the first notch to drive a second push block to move towards the two ends of the first filter plate, the second push block pushes a third push block in a rotating block to separate a clamping block from a second notch of the first stop block, so that the first filter plate is overturned due to the weight of zirconium tetrachloride precipitate on the surface, the rotating block drives the first filter plate to rotate 180 degrees under the action of inertia, meanwhile, the air bag drives the first push block to move downwards due to the falling of the liquid level, the second push block is separated from the third push block, and the clamping block is clamped in the first notch on the surface of the first stop block, the position of the first filter plate in the machine shell is fixed, so that the effect of preventing the first filter plate from being blocked is achieved.
2. This method to crude zirconium tetrachloride purification kind recovery aluminium chloride, through the inside temperature of thermistor control reaction chamber, thermistor and electromagnetic means electric connection, the produced magnetic field magnetic pole of electromagnetic means is opposite with opposite face third magnetic path magnetic pole, electromagnetic means is driving the second metal ball through the third magnetic path and is sliding on the varistor, thereby change the resistance value of varistor, the power of heater in the control reaction chamber, thereby prevent that the high temperature from leading to aluminium chloride sublimation or the low temperature leads to carbon tetrachloride can not volatilize, thereby reached the effect of automatic control temperature.
Drawings
FIG. 1 is a schematic view of the overall structure of the recycling apparatus of the present invention;
FIG. 2 is a schematic view of the structure at A in FIG. 1;
FIG. 3 is a schematic view of the structure at B in FIG. 1;
FIG. 4 is an enlarged view of the second pushing block in the moving state according to the present invention;
FIG. 5 is a schematic view of the structure of FIG. 1 at C;
fig. 6 is a schematic structural diagram at D in fig. 1.
In the figure: 1. a housing; 2. a drive shaft; 3. a first long rod; 4. a second long rod; 5. a feed pipe; 6. a switching device; 601. a first notch; 602. a first push block; 603. a metal block; 604. an air bag; 605. a first metal ball; 606. a second push block; 607. a first stopper; 608. a second notch; 7. a first filter plate; 8. rotating the block; 9. a third push block; 10. a clamping block; 11. a second filter plate; 12. drawing a pipe; 13. a reaction chamber; 1301. a heater; 1302. a collection plate; 1303. a first magnetic block; 1304. a second magnetic block; 1305. a second stopper; 1306. a thermistor; 14. a control device; 1401. an electromagnetic device; 1402. a third magnetic block; 1403. a second metal ball; 1404. a variable resistor; 15. a water tank; 16. a cooling device; 17. and collecting the tubes.
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.
A method for recovering aluminum chloride from crude zirconium tetrachloride purification seeds comprises the following steps:
s1, firstly, introducing crude zirconium tetrachloride containing aluminum chloride impurities into a carbon tetrachloride solution, dissolving aluminum chloride in carbon tetrachloride by stirring, controlling the rotating speed to operate at 30 revolutions per minute, and precipitating the zirconium tetrachloride at the bottom of the carbon tetrachloride solution;
s2, evaporating the carbon tetrachloride solution on the surface of the zirconium tetrachloride when the temperature of the left end outlet of the heating furnace is between 78 and 170 ℃, and discharging the zirconium tetrachloride out of the furnace in an extraction mode;
s3; and finally, heating the indoor temperature to 90-170 ℃ by utilizing the difference of the boiling points of the carbon tetrachloride and the aluminum chloride, volatilizing the carbon tetrachloride indoors, and heating the aluminum chloride into white particles to precipitate on the indoor bottom end.
Referring to fig. 1-6, according to the method for recovering aluminum chloride from a crude zirconium tetrachloride purification seed according to claim 1, there is provided an apparatus for recovering aluminum chloride from a crude zirconium tetrachloride purification seed, which includes a housing 1, a driving shaft 2 rotatably connected to the middle of the housing 1, a first long rod 3 rotatably connected to the lower end of the driving shaft 2, a second long rod 4 provided at the bottom end of the first long rod 3, feed pipes 5 provided at both sides of the housing 1, a switch device 6 provided at the bottom end of the feed pipes 5, a first notch 601 formed inside the switch device 6, a first push block 602 slidably connected inside the housing 1 and in the first notch 601, a metal block 603 fixedly connected inside the first push block 602, an air bag 604 fixedly connected to the bottom end of the first push block 602, a first metal ball 605 provided at the lower end of the air bag 604, and a second push block 606 provided inside the housing 1 and at an end of the first notch 601 far from the first push block 602.
The second pushing block 606 is connected in the first notch 601 in a sliding manner, the air bag 604 drives the first pushing block 602 to slide in the first notch 601 when the liquid level rises, the air in the first notch 601 is extruded, the second pushing block 606 slides in the first notch 601, one end of the second pushing block 606 far away from the first pushing block 602 is provided with a first stop 607, the surface of the first stop 607 is provided with a second notch 608, the bottom end of the second long rod 4 is provided with a first filter plate 7, two ends of the first filter plate 7 are fixedly connected with rotating blocks 8, the inside of the rotating block 8 is connected with a third pushing block 9 in a sliding manner, a clamping block 10 fixedly connected on the surface of the third pushing block 9 is matched with the second notch 608 arranged on the surface of the first stop 607, the third pushing block 9 is pushed by the second pushing block 606, the clamping block 10 is separated from the second notch 608, the rotating block 8 drives the first filter plate 7 to rotate, and the clamping block 10 is connected in a sliding manner inside the third pushing block, the bottom end of the first filter plate 7 is provided with a second filter plate 11.
The second filter plate 11 is obliquely arranged in the machine case 1 to accelerate the sliding speed of zirconium tetrachloride on the second filter plate 11, meanwhile, the mixed liquid of carbon tetrachloride and aluminum chloride has a pushing effect on zirconium tetrachloride, the left side of the second filter plate 11 is provided with a pipe 12, the right side of the second filter plate 11 is provided with a reaction chamber 13, the inside of the reaction chamber 13 is fixedly connected with a heating wire 1301, the upper end of the heating wire 1301 is provided with a collecting plate 1302, the left side of the collecting plate 1302 is fixedly connected with a first magnetic block 1303, the magnetic pole of the first magnetic block 1303 is opposite to the magnetic pole of a second magnetic block 1304 opposite to each other, the second magnetic block 1304 is fixed in the second magnetic block 1305, the collecting plate 1302 can control the second magnetic block 1305 to slide up and down in the reaction chamber 13 through the first magnetic block 1303, the upper part of the first magnetic block 1303 is provided with a second magnetic block 1304, the surface of the, the thermistor 1306 is electrically connected with the electromagnetic device 1401, and the magnetic pole of the magnetic field generated by the electromagnetic device 1401 is the same as the magnetic pole of the third magnetic block 1402 opposite to the magnetic pole.
The electromagnetic device 1401 drives a second metal ball 1403 to slide on the variable resistor 1404 by a third magnetic block 1402, the upper end of the reaction chamber 13 is fixedly connected with a control device 14, the electromagnetic device 1401 is fixedly connected inside the control device 14, the third magnetic block 1402 is arranged on the right side of the electromagnetic device 1401, the surface of the third magnetic block 1402 is fixedly connected with the second metal ball 1403, the second metal ball 1403 is connected with the variable resistor 1404 in a sliding mode, a water tank 15 is arranged on the right side of the control device 14, a cooling device 16 is arranged on the upper portion of the water tank 15, and a collecting pipe 17 is arranged on the right side of the.
When the device is used, firstly, zirconium tetrachloride containing aluminum chloride impurities is poured into the interior of the machine shell 1 from the feeding pipe 5 on the left side of the machine shell 1, a carbon tetrachloride solution is input into the interior of the machine shell 1 from the feeding pipe 5 on the right side of the machine shell 1, according to the principle that the zirconium tetrachloride cannot be dissolved in the carbon tetrachloride solution and the aluminum chloride can be dissolved, the first long rod 3 is driven by the driving shaft 2 to rotate in the interior of the machine shell 1, the first long rod 3 drives the second long rod 4 to stir materials on the first filter plate 7, the solution flows downwards through filter holes on the first filter plate 7, the zirconium tetrachloride and the undissolved aluminum chloride are remained on the surface of the first filter plate 7, the second long rod 4 not only stirs the zirconium tetrachloride and the aluminum chloride on the surface of the first filter plate 7, but also cleans the zirconium tetrachloride and the aluminum chloride attached to the inner wall of the machine shell 1 by.
When the zirconium tetrachloride on the surface of the first filter plate 7 is too much, the zirconium tetrachloride will block the filter holes of the first filter plate 7, so that the liquid level of the carbon tetrachloride in the casing 1 rises, the rising liquid level pushes the air bag 604 in the first notch 601 to move upwards, the surface of the air bag 604 is fixedly connected with the first push block 602, the surface of the first push block 602 adopts rubber material, the air in the first notch 601 is pushed by the first push block 602 to drive the second push block 606 to move towards the two ends of the first push block 602, the third pushing block 9 in the rotating block is pushed by the second pushing block 606, so that the clamping block 10 on the surface of the third pushing block 9 is separated from the second notch 608 of the first clamping block 607, thereby the first filter plate 7 is overturned due to the weight of the zirconium tetrachloride deposit on the surface, the rotating block 8 drives the first filter plate 7 to rotate 180 degrees under the action of inertia, while the zirconium tetrachloride precipitate falls off from the surface of the first filter plate 7 onto the second filter plate 11.
Because the second filter plate 11 is obliquely arranged in the machine shell 1, the zirconium tetrachloride is pushed to slide to the left end of the machine shell 1, the temperature of the position of the pumping pipe 12 is adjusted to 78-170 ℃ by heating the heating wire 1301, so that the carbon tetrachloride solution on the surface of the zirconium tetrachloride is evaporated and moves upwards, meanwhile, the airbag 604 drives the metal block 603 on the first push block 602 to contact with the first metal ball 605 due to the liquid level reduction, the pumping pipe 12 is opened, the zirconium tetrachloride slides out of the pumping pipe 12 for collection, the second push block 606 is separated from the third push block 9, the fixture block 10 is clamped in the first notch 601 on the surface of the first stop block 607, the position of the first filter plate 7 in the machine shell 1 is fixed, and the effect of separating the zirconium tetrachloride and the aluminum chloride is achieved.
Secondly, the mixed liquid of carbon tetrachloride and aluminum chloride flows into the reaction chamber 13, the collecting plate 1302 is shifted to the right side, so that the first magnetic block 1303 can not move the second block 1305 upwards through the second magnetic block 1304, the magnetic pole of the first magnetic block 1303 is opposite to that of the second magnetic block 1304 opposite to the first magnetic block, so that the second block 1305 blocks the inlet of the reaction chamber 13 due to the weight of the second block, the temperature in the reaction chamber is increased to 90-170 ℃ through heating of a heating wire, carbon tetrachloride enters the collecting pipe 17 through volatilization according to the difference of the boiling points between the carbon tetrachloride and the aluminum chloride, and then returns to the feeding pipe 5 through the cooling device 16, the collecting pipe 17 in the cooling device 16 is inclined, and the carbon tetrachloride enters the feeding pipe 5 on the right side of the.
Meanwhile, aluminum chloride is heated into white particles to be deposited on the surface of the collecting plate 1302, the temperature inside the reaction chamber 13 is controlled and controlled through the thermistor 1306, the thermistor 1306 is electrically connected with the electromagnetic device 1401, the magnetic pole of a magnetic field generated by the electromagnetic device 1401 is opposite to the magnetic pole of the third magnetic block 1402 opposite to the magnetic pole, the electromagnetic device 1401 drives the second metal ball 1403 to slide on the variable resistor 1404 through the third magnetic block 1402, so that the resistance value of the variable resistor 1404 is changed, the power of the heating wire 1301 in the reaction chamber 13 is controlled, and therefore the aluminum chloride is prevented from sublimating due to overhigh temperature or carbon tetrachloride cannot volatilize due to overlow temperature, and waste of resources is avoided.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A method for recovering aluminum chloride from a crude zirconium tetrachloride purification seed is characterized by comprising the following steps:
s1, firstly, introducing crude zirconium tetrachloride containing aluminum chloride impurities into a carbon tetrachloride solution, dissolving aluminum chloride in carbon tetrachloride by stirring, controlling the rotating speed to operate at 30 revolutions per minute, and precipitating the zirconium tetrachloride at the bottom of the carbon tetrachloride solution;
s2, evaporating the carbon tetrachloride solution on the surface of the zirconium tetrachloride when the temperature of the left end outlet of the heating furnace is between 78 and 170 ℃, and discharging the zirconium tetrachloride out of the furnace in an extraction mode;
s3; and finally, heating the indoor temperature to 90-170 ℃ by utilizing the difference of the boiling points of the carbon tetrachloride and the aluminum chloride, volatilizing the carbon tetrachloride indoors, and heating the aluminum chloride into white particles to precipitate on the indoor bottom end.
2. The method for recovering aluminum chloride from crude zirconium tetrachloride purification seeds according to claim 1, which provides an aluminum chloride recovery device from crude zirconium tetrachloride purification seeds, characterized by comprising a machine shell (1), and characterized in that: the middle of the machine shell (1) is rotatably connected with a driving shaft (2), the lower end of the driving shaft (2) is rotatably connected with a first long rod (3), the bottom end of the first long rod (3) is provided with a second long rod (4), two sides of the machine shell (1) are provided with feeding pipes (5), the bottom end of the feeding pipe (5) is provided with a switch device (6), a first notch (601) is formed in the switch device (6), a first push block (602) is connected in the machine shell (1) in a sliding mode in the first notch (601), a metal block (603) is fixedly connected in the first push block (602), the bottom end of the first push block (602) is fixedly connected with an air bag (604), a first metal ball (605) is arranged at the lower end of the air bag (604), and a second push block (606) is arranged in the machine shell (1) and at one end, far away from the first push block (602), a first stop block (607) is arranged at one end, far away from the first push block (602), of the second push block (606), a second notch (608) is formed in the surface of the first stop block (607), a first filter plate (7) is arranged at the bottom end of the second long rod (4), rotating blocks (8) are fixedly connected to two ends of the first filter plate (7), a third push block (9) is slidably connected to the inside of each rotating block (8), a clamping block (10) is slidably connected to the inside of each third push block (9), a second filter plate (11) is arranged at the bottom end of the first filter plate (7), a pumping pipe (12) is arranged at the left side of each second filter plate (11), a reaction chamber (13) is arranged at the right side of each second filter plate (11), a heating wire (1301) is fixedly connected to the inside of each reaction chamber (13), a collecting plate (1302) is arranged at the upper end of each heating wire (1301), and a first magnetic block (1303), the improved reactor is characterized in that a second magnetic block (1304) is arranged on the upper portion of the first magnetic block (1303), a second stopper (1305) is fixedly connected to the surface of the second magnetic block (1304), thermistors (1306) are fixedly connected to the two sides of the reaction chamber (13), a control device (14) is fixedly connected to the upper end of the reaction chamber (13), an electromagnetic device (1401) is fixedly connected to the inside of the control device (14), a third magnetic block (1402) is arranged on the right side of the electromagnetic device (1401), a second metal ball (1403) is fixedly connected to the surface of the third magnetic block (1402), a variable resistor (1404) is slidably connected to the second metal ball (1403), a water tank (15) is arranged on the right side of the control device (14), a cooling device (16) is arranged on the upper portion of the water tank (15), and a collecting pipe.
3. The apparatus for recovering aluminum chloride from a crude zirconium tetrachloride purification seed as claimed in claim 2, wherein: the second push block (606) is connected in a sliding mode inside the first notch (601).
4. The apparatus for recovering aluminum chloride from a crude zirconium tetrachloride purification seed as claimed in claim 2, wherein: a clamping block (10) fixedly connected to the surface of the third pushing block (9) is matched with a second notch (608) formed in the surface of the first clamping block (607).
5. The apparatus for recovering aluminum chloride from a crude zirconium tetrachloride purification seed as claimed in claim 2, wherein: the second filter plate (11) is obliquely arranged inside the machine shell (1).
6. The apparatus for recovering aluminum chloride from a crude zirconium tetrachloride purification seed as claimed in claim 2, wherein: the thermistor (1306) is electrically connected with the electromagnetic device (1401).
7. The apparatus for recovering aluminum chloride from a crude zirconium tetrachloride purification seed as claimed in claim 2, wherein: the magnetic pole of the first magnetic block (1303) is opposite to that of the second magnetic block (1304) opposite to the magnetic pole of the first magnetic block.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010991513.9A CN112206729A (en) | 2020-11-24 | 2020-11-24 | Method for recovering aluminum chloride by aiming at crude zirconium tetrachloride purification seeds |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010991513.9A CN112206729A (en) | 2020-11-24 | 2020-11-24 | Method for recovering aluminum chloride by aiming at crude zirconium tetrachloride purification seeds |
Publications (1)
Publication Number | Publication Date |
---|---|
CN112206729A true CN112206729A (en) | 2021-01-12 |
Family
ID=74050211
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202010991513.9A Pending CN112206729A (en) | 2020-11-24 | 2020-11-24 | Method for recovering aluminum chloride by aiming at crude zirconium tetrachloride purification seeds |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112206729A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112973215A (en) * | 2021-02-23 | 2021-06-18 | 玉良(山东)贸易有限公司 | Intelligent anti-overflow water treatment equipment based on horizontal plane change |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4737244A (en) * | 1986-12-18 | 1988-04-12 | Westinghouse Electric Corp. | Zirconium and hafnium tetrachloride separation by extractive distillation with molten zinc chloride lead chloride solvent |
CN109809483A (en) * | 2017-11-20 | 2019-05-28 | 王鹏 | A kind of thick zirconium chloride impurity removal and purification technique |
CN109809484A (en) * | 2017-11-20 | 2019-05-28 | 田长对 | A method of high-purity zirconium chloride is prepared using sodium hydroxide |
CN110697659A (en) * | 2019-08-12 | 2020-01-17 | 中国石油大学(华东) | Method for separating and extracting sulfur powder in water in insoluble sulfur preparation process |
CN111686473A (en) * | 2019-03-13 | 2020-09-22 | 北京石油化工学院 | Method for separating iron oxide waste desulfurizer from sulfur |
-
2020
- 2020-11-24 CN CN202010991513.9A patent/CN112206729A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4737244A (en) * | 1986-12-18 | 1988-04-12 | Westinghouse Electric Corp. | Zirconium and hafnium tetrachloride separation by extractive distillation with molten zinc chloride lead chloride solvent |
CN109809483A (en) * | 2017-11-20 | 2019-05-28 | 王鹏 | A kind of thick zirconium chloride impurity removal and purification technique |
CN109809484A (en) * | 2017-11-20 | 2019-05-28 | 田长对 | A method of high-purity zirconium chloride is prepared using sodium hydroxide |
CN111686473A (en) * | 2019-03-13 | 2020-09-22 | 北京石油化工学院 | Method for separating iron oxide waste desulfurizer from sulfur |
CN110697659A (en) * | 2019-08-12 | 2020-01-17 | 中国石油大学(华东) | Method for separating and extracting sulfur powder in water in insoluble sulfur preparation process |
Non-Patent Citations (3)
Title |
---|
《稀有金属手册》编辑委员会编著: "《稀有金属手册 下》", 31 December 1995, 冶金工业出版社 * |
吕世光: "《塑料橡胶助剂手册》", 30 September 1995, 中国轻工业出版社 * |
吴景梅等: "《有机化学实验》", 30 September 2016, 安徽大学出版社 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112973215A (en) * | 2021-02-23 | 2021-06-18 | 玉良(山东)贸易有限公司 | Intelligent anti-overflow water treatment equipment based on horizontal plane change |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
KR101440208B1 (en) | Vertical countercurrent solid-liquid contact method, method for washing solid particles, method for producing polyarylene sulfide, and device therefor | |
CN112206729A (en) | Method for recovering aluminum chloride by aiming at crude zirconium tetrachloride purification seeds | |
CN105197904A (en) | Continuous drying system for three-waste comprehensive recovery treatment | |
CN110342774A (en) | A kind of drying method for sludge | |
CN103627913B (en) | Purification and recovery method for tin slag and recovery apparatus | |
CN104968464A (en) | Apparatus and method for solder recovery | |
CN106745250A (en) | Aoxidize the device and piece of Vanadium production method of powdery vanadic anhydride | |
CN106839739B (en) | The working method of continuous drying system for chemical residual liquor processing | |
CN100586526C (en) | Method and apparatus for processing suspension | |
CN212680083U (en) | Explosion-proof solvent recovery machine for treating and purifying high-viscosity materials | |
CN211963125U (en) | Distillation recovery device for polyarylate production | |
CN210426057U (en) | Scrap recovery device for aluminum alloy production | |
CN215388073U (en) | Filter device in silver electrolysis equipment | |
CN211199359U (en) | Zinc oxide recovery refining equipment | |
CN106591598A (en) | Arsenic trioxide sublimation purifying furnace for floating body fine control by low-melting-point alloy | |
CN215828554U (en) | A recovery unit that is used for high salt waste liquid to carry iodine | |
CN214562104U (en) | Production plastic pellet is with compounding bucket that has unloading volume control structure | |
CN212914803U (en) | Solvent refining plant is used in rubber plasticizer production and processing | |
CN103913050B (en) | The continuous drier of slurry or powder | |
CN211752961U (en) | Coating filters cooling device | |
CN216890229U (en) | Device for recycling nickel in chemical nickel waste liquid | |
CN217962404U (en) | Benzethonium chloride preparation mixing arrangement | |
CN213726512U (en) | Tetrafluoroterephthalonitrile high efficiency filter desalination separator | |
CN211384050U (en) | Filter equipment that chemistry chemical industry was used | |
CN212955278U (en) | Enrichment recovery unit of iridium in iridium-containing sand |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210112 |