CN116161621B - Purification device and purification process of electronic grade hydrochloric acid - Google Patents
Purification device and purification process of electronic grade hydrochloric acid Download PDFInfo
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- CN116161621B CN116161621B CN202310441919.3A CN202310441919A CN116161621B CN 116161621 B CN116161621 B CN 116161621B CN 202310441919 A CN202310441919 A CN 202310441919A CN 116161621 B CN116161621 B CN 116161621B
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- hydrochloric acid
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- exchange column
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 213
- 238000000746 purification Methods 0.000 title claims abstract description 31
- 230000007246 mechanism Effects 0.000 claims abstract description 61
- 238000001179 sorption measurement Methods 0.000 claims abstract description 27
- 239000011347 resin Substances 0.000 claims abstract description 15
- 229920005989 resin Polymers 0.000 claims abstract description 15
- 238000011010 flushing procedure Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000005540 biological transmission Effects 0.000 claims description 55
- 230000033001 locomotion Effects 0.000 claims description 15
- 230000003247 decreasing effect Effects 0.000 claims description 3
- 230000002035 prolonged effect Effects 0.000 claims description 2
- USYLIGCRWXYYPZ-UHFFFAOYSA-N [Cl].[Fe] Chemical compound [Cl].[Fe] USYLIGCRWXYYPZ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 description 12
- 230000003068 static effect Effects 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- 230000000712 assembly Effects 0.000 description 2
- 238000000429 assembly Methods 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
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- 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
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0718—Purification ; Separation of hydrogen chloride by adsorption
-
- 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
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
-
- 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
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0731—Purification ; Separation of hydrogen chloride by extraction
- C01B7/0737—Purification ; Separation of hydrogen chloride by extraction hydrogen chloride being extracted
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to the field of hydrochloric acid preparation, and discloses a purification device and a purification process of electronic grade hydrochloric acid, wherein the purification device comprises a hydrochloric acid feeding mechanism, a hydrochloric acid adsorption mechanism and a hydrochloric acid rectifying mechanism which are sequentially arranged; the hydrochloric acid adsorption mechanism comprises exchange columns and flushing components, wherein the exchange columns are distributed in a circumferential array around the upright columns, the upright columns are arranged vertically, adsorption resin is filled in each exchange column, two ends of each exchange column are provided with pipe joints, the two pipe joints are connected with the flushing components through water pipes, hydrochloric acid connectors are arranged on the column bodies of the exchange columns, one hydrochloric acid connector is connected with the hydrochloric acid feeding mechanism, and the other hydrochloric acid connector is connected with the hydrochloric acid rectifying mechanism; the purification device provided by the invention can realize the function of carrying out the association automation of adsorption and removal of the iron-chlorine complex compound on the industrial hydrochloric acid, has high adsorption efficiency, can realize the rapid flushing regeneration of the resin in the exchange column, and meets the requirement of large-scale and high-efficiency purification of the electronic grade hydrochloric acid.
Description
Technical Field
The invention relates to the field of hydrochloric acid preparation, in particular to a purification device and a purification process of electronic grade hydrochloric acid.
Background
The electronic grade hydrochloric acid is colorless transparent hydrogen chloride aqueous solution, has strong corrosiveness and strong acidity, and has wider application range, but is difficult to prepare, and most of the hydrochloric acid in China depends on import.
At present, the electronic grade hydrochloric acid is generally prepared by purifying and refining industrial grade hydrochloric acid as a raw material, the purification process is generally to remove the iron-chlorine complex in the hydrochloric acid firstly, then purifying and treating the hydrochloric acid by means of rectification and the like, and how to continuously and automatically and efficiently remove the iron-chlorine complex in the industrial hydrochloric acid is an urgent problem to be solved in the large-scale preparation of the electronic grade hydrochloric acid at present.
Disclosure of Invention
In order to solve the technical problems, the invention provides a purification device and a purification process of electronic grade hydrochloric acid.
The purifying device of the electronic grade hydrochloric acid comprises a hydrochloric acid feeding mechanism, a hydrochloric acid adsorption mechanism and a hydrochloric acid rectifying mechanism which are sequentially arranged;
the hydrochloric acid adsorption mechanism comprises exchange columns and flushing components, wherein the exchange columns are distributed in a circumferential array around the upright columns, the upright columns are arranged vertically, adsorption resin is filled in each exchange column, two ends of each exchange column are provided with pipe joints, the two pipe joints are connected with the flushing components through water pipes, hydrochloric acid connectors are arranged on the column bodies of the exchange columns, one hydrochloric acid connector is connected with the hydrochloric acid feeding mechanism, and the other hydrochloric acid connector is connected with the hydrochloric acid rectifying mechanism;
each exchange column is arranged on a supporting mechanism, and the supporting mechanism comprises supporting components which are arranged in a one-to-one correspondence manner;
the vertically distributed exchange columns are marked as A-state exchange columns;
the exchange columns which are horizontally distributed are marked as B-state exchange columns;
the A-state exchange columns and the B-state exchange columns are alternately distributed around the upright columns, the supporting component is connected with the switching mechanism, the switching mechanism is used for adjusting the mutual switching of the A-state exchange columns and the B-state exchange columns, each exchange column is connected with the adjusting mechanism, and the adjusting mechanism is used for adjusting the shaking and/or the swaying of the exchange columns.
The support assembly comprises an A assembly and a B assembly, the A assembly comprises two hoop frames and an A rectangular rod group, the two hoop frames are fixedly arranged at two ends of the exchange column, the A rectangular rod group comprises two parallel A1 rods and two parallel A2 rods, the two A1 rods and the two A2 rods enclose a rectangle, the A1 rods are arranged along the length direction of the exchange column, the two A2 rods are respectively arranged at two ends of the A1 rods, the ends of the A1 rods and the ends of the A2 rods are hinged through an A hinge shaft, the planes of the A hinge shaft, the A1 rods and the A2 rods are vertical, the two A2 rods are fixedly connected with the two hoop frames respectively, the A adjusting mechanism comprises an A adjusting assembly and a B adjusting assembly, the A adjusting assembly is connected with the A1 rods close to the exchange column, and the A adjusting assembly is used for adjusting the A1 rods close to the exchange column to reciprocate along the length direction of the other A1 rods.
The B component comprises two groups of B rectangular rod groups, the two groups of B rectangular rod groups are arranged at two ends far away from the A1 rod, the B rectangular rod groups comprise two parallel-distributed B1 rods and two parallel-distributed B2 rods, the two B1 rods and the two B2 rods enclose a rectangle, the plane where the two B1 rods and the B2 rods are located is perpendicular to the A1 rod, the end parts of the B1 rods and the B2 rods are hinged through a B hinge shaft, the B1 rods and the A1 rods are vertically distributed, the two B2 rods are radially distributed at intervals along the exchange column, one B1 rod is recorded as a supporting rod, one end of the supporting rod is prolonged and is rotationally connected with the A hinge shaft, the B2 rod far away from the exchange column is connected with a B adjusting component, and the B adjusting component is used for adjusting the rotation of the B2 rod around the B hinge shaft.
The B adjusting component comprises a supporting cylinder and a transmission shaft, the supporting cylinder is arranged along the length direction of the rod of the A1 rod, the two B2 rods are fixedly connected with rotating shafts, the axial direction of the rotating shafts is consistent with the length direction of the rod of the A1 rod, the two rotating shafts are rotatably arranged at two ends of the supporting cylinder, the transmission shaft and the B1 rod are distributed in parallel, one end of the transmission shaft is rotatably arranged in the supporting cylinder, and one rotating shaft is connected with the transmission shaft through the B transmission component and the selection component.
The A adjusting component comprises a swing arm, the middle part of the swing arm is rotatably installed on an A1 rod far away from the exchange column through a first hinge shaft, a cylindrical pin is fixedly installed on the A1 rod close to the exchange column, the axial directions of the first hinge shaft and the cylindrical pin are consistent, the axial direction of the first hinge shaft is perpendicular to the length direction of the rod of the A1 rod, a guide groove is formed in the swing arm along the length direction of the arm, the cylindrical pin is slidably installed in the guide groove, and the other end of the swing arm is connected with a transmission shaft through an A transmission component and a selection component.
The A transmission assembly comprises a first supporting rod and a second supporting rod, one end of the first supporting rod is hinged to one end of the swing arm far away from the cylindrical pin through a second hinge shaft, the other end of the first supporting rod is hinged to one end of the second supporting rod through a third hinge shaft, the second hinge shaft is consistent with the axial direction of the shaft length of the A1 rod, the other end of the second supporting rod is connected with arc teeth, the circle center of each arc tooth is located on the axis of the first hinge shaft, the arc teeth are meshed with racks, the racks are arranged along the length direction of the supporting cylinder, the racks are slidably mounted on the outer wall of the supporting cylinder along the length direction of the rack, constraint components are mounted on the outer wall of the supporting cylinder and are correspondingly arranged with the arc teeth, and the constraint components are used for constraining the arc teeth to move along the thickness direction of the arc teeth and are connected with the selection assembly through the linkage components.
The restraint subassembly includes two baffles, and two baffles and arc tooth both sides sliding fit all offer the arc wall on two baffles, and the centre of a circle of arc wall is located the axis of first articulated shaft, and arc tooth both sides set up the sliding pin, and sliding pin slidable mounting is in the arc wall.
The linkage assembly is arranged in the supporting cylinder and comprises a sliding block and a linkage shaft, the linkage shaft and the transmission shaft are arranged along the extension direction, the shaft body of the linkage shaft is rotatably arranged in the supporting cylinder, the sliding block is fixedly connected with the rack, a sliding groove is formed in the sliding block, the groove direction of the sliding groove is perpendicular to the length direction of the rack, one end, close to the sliding block, of the linkage shaft is fixedly connected with one end of the linkage arm, the linkage arm and the linkage shaft are vertically distributed, a pin shaft is arranged at one end, far away from the linkage shaft, of the linkage arm, and the pin shaft is slidably arranged in the sliding groove.
The transmission assembly B comprises a hollow shaft, the hollow shaft is sleeved on the transmission shaft, an A bevel gear is arranged on the hollow shaft, a B bevel gear is arranged at the end part of the rotation shaft, and the A bevel gear is meshed with the B bevel gear.
The selection component comprises two sliding shafts which are sleeved on the transmission shaft, the two sliding shafts and the transmission shaft form sliding guide fit along the axial direction of the transmission shaft, two ends of the two sliding shafts respectively correspond to the end parts of the hollow shaft and the linkage shaft, the corresponding end parts of the two sliding shafts, the hollow shaft and the linkage shaft are of a saw-tooth structure, the two sliding shafts are connected with the selection unit, and the selection unit is used for adjusting the two sliding shafts to slide along the axial direction of the transmission shaft so as to be connected with the hollow shaft and/or the linkage shaft.
The end parts of the two sliding shafts, which are close to each other, are provided with annular plates, the surfaces of the two annular plates, which are close to each other, are inclined surfaces, the selection unit comprises a first deflector rod, a separation fork rod and a second deflector rod, the first deflector rod and the second deflector rod are respectively propped against the surfaces of the two annular plates, which are away from each other, the separation fork rod points to a position between the two annular plates, the end parts of the separation fork rod are wedge blocks, the first deflector rod and the second deflector rod are respectively connected with corresponding reciprocating components, the reciprocating components are used for adjusting the axial movement of the first deflector rod or the second deflector rod along a transmission shaft, the separation fork rod is connected with a telescopic component, and the telescopic component is used for adjusting the telescopic movement of the separation fork rod; the reciprocating assembly and the telescopic assembly are both air cylinders, so that the movement of the first deflector rod and the second deflector rod can be pneumatically regulated, and the telescopic movement of the separation fork rod can be regulated.
A C-shaped bevel gear is arranged at one end of the transmission shaft, which is far away from the exchange column, and a conical fluted disc is rotatably arranged on the upright post, and each C-shaped bevel gear is meshed with the conical fluted disc.
The switching mechanism comprises a limiting block, a limiting sleeve shaft and a switching unit, wherein the limiting block is fixedly installed, the limiting sleeve shaft is sleeved on the transmission shaft, one end of the limiting sleeve shaft is fixedly connected with the supporting cylinder, a passive rod is installed at one end of the limiting sleeve shaft, which is far away from the supporting cylinder, the limiting sleeve shaft is inserted in the limiting block, the outer wall of the limiting sleeve shaft is provided with a strip-shaped bulge, and a groove matched with the strip-shaped bulge is formed in the limiting block;
the switching unit is correspondingly arranged with each passive rod, and is used for abutting against the passive rod to drive the limiting sleeve shaft to extend out of the limiting block, and after the protrusion is separated from the groove, the switching unit drives the passive rod to drive the limiting sleeve shaft to rotate ninety degrees, so that the A-state exchange column is switched into the B-state exchange column; similarly, the switching unit toggles the driven rod to reset, then the driven rod is adjusted to retract, the limiting sleeve shaft is driven to return to the original position, and the switching of the B-state switching column into the A-state switching column is realized.
A purification process of electronic grade hydrochloric acid comprises the following steps:
s1: preparing two groups of exchange columns, namely a group A and a group B, wherein each exchange column in the group A is vertically distributed, each exchange column in the group B is horizontally distributed, and the group A and the group B can be mutually switched;
s2: each exchange column in the group A is sequentially divided into two groups, each exchange column in the front group has decreasing motion freedom degree and amplitude, each exchange column in the rear group is vertically stationary, and then hydrochloric acid is introduced into each exchange column in each group A one by one;
s3: after hydrochloric acid is introduced into the A group exchange column for a preset time, the A group is switched into the B group, the B group is switched into the A group, and hydrochloric acid is introduced into the newly switched A group exchange column;
s4: and (3) eluting and reducing the resin in the group B exchange column.
The invention has the beneficial effects that: the purification device provided by the invention can realize the function of carrying out the association automation of adsorption and removal of the iron-chlorine complex compound on the industrial hydrochloric acid, has high adsorption efficiency, can realize the rapid flushing regeneration of the resin in the exchange column, and meets the requirement of large-scale and high-efficiency purification of the electronic grade hydrochloric acid.
Drawings
FIG. 1 is a schematic diagram of the purification device of electronic grade hydrochloric acid;
FIG. 2 is a schematic top view of a hydrochloric acid adsorption mechanism in an electronic grade hydrochloric acid purification device according to the present invention;
FIG. 3 is a schematic view of a fluted disc in a hydrochloric acid adsorption mechanism in an electronic grade hydrochloric acid purifying device;
FIG. 4 is a schematic diagram of the structure of a single column in the hydrochloric acid adsorption mechanism in an electronic grade hydrochloric acid purification device;
FIG. 5 is a schematic structural view of a supporting mechanism in a hydrochloric acid adsorbing mechanism in an electronic grade hydrochloric acid purifying device;
FIG. 6 is a schematic diagram of the structure of racks and arc teeth in the hydrochloric acid adsorption mechanism in the purification device of electronic grade hydrochloric acid;
fig. 7 is a schematic structural diagram of a selective component in a hydrochloric acid adsorption mechanism in a purification device of electronic grade hydrochloric acid.
In the figure: 1. a hydrochloric acid feeding mechanism; 2. a hydrochloric acid adsorption mechanism; 3. hydrochloric acid rectifying mechanism; 4. a flushing assembly;
100. an exchange column; 110. a pipe joint; 120. a hydrochloric acid joint; 200. a support mechanism; 210. an A component; 211. a1, a rod; 212. a2, a rod; 213. a is a hinge shaft; 220. a component B; 221. b1 bar; 222. a B2 rod; 223. a hinge shaft B; 300. an adjusting mechanism; 310. an A adjusting component; 311. swing arms; 312. a cylindrical pin; 313. a first hinge shaft; 314. a first strut; 315. a second strut; 316. arc teeth; 317. a sliding pin; 318. a rack; 319. a baffle; 320. a B adjusting component; 321. a support cylinder; 322. a rotating shaft; 323. a bevel gear B; 324. a bevel gear; 325. a hollow shaft; 330. a transmission shaft; 331. c bevel gear; 340. a selection component; 341. a sliding shaft; 342. an annular plate; 343. a first deflector rod; 344. a second deflector rod; 345. separating fork bars; 350. a linkage assembly; 351. a linkage shaft; 352. a linkage arm; 353. a pin shaft; 354. a slide block; 360. conical fluted disc; 400. a switching mechanism; 410. a limiting block; 420. a limiting sleeve shaft; 430. a passive lever; 500. and (5) a column.
Detailed Description
The subject matter described herein will now be discussed with reference to example embodiments. It is to be understood that these embodiments are merely discussed so that those skilled in the art may better understand and implement the subject matter described herein and that changes may be made in the function and arrangement of the elements discussed without departing from the scope of the disclosure herein. Various examples may omit, replace, or add various procedures or components as desired. In addition, features described with respect to some examples may be combined in other examples as well.
Example 1
Referring to fig. 1 to 7, in this embodiment, a purification apparatus for electronic grade hydrochloric acid is provided, which includes a hydrochloric acid feeding mechanism 1, a hydrochloric acid adsorbing mechanism 2, and a hydrochloric acid rectifying mechanism 3 arranged in this order;
the hydrochloric acid adsorption mechanism 2 comprises exchange columns 100 and flushing assemblies 4, wherein the exchange columns 100 are distributed in a circumferential array around a column 500, the column 500 is arranged vertically, adsorption resin is filled in each exchange column 100, pipe joints 110 are arranged at two ends of each exchange column 100, the two pipe joints 110 are connected with the flushing assemblies 4 through water pipes, hydrochloric acid joints 120 are arranged on the column bodies of the exchange columns 100, one hydrochloric acid joint 120 is connected with the hydrochloric acid feeding mechanism 1, and the other hydrochloric acid joint 120 is connected with the hydrochloric acid rectifying mechanism 3;
each exchange column 100 is mounted on a supporting mechanism 200, and the supporting mechanism 200 comprises each supporting component, and each supporting component and each exchange column 100 are arranged in a one-to-one correspondence manner;
the vertically distributed exchange column is denoted as an a-state exchange column 100;
the horizontally distributed exchange column is denoted as a B-state exchange column 100;
the A-state exchange columns and the B-state exchange columns are alternately distributed around the upright 500, the support component is connected with the switching mechanism 400, the switching mechanism 400 is used for adjusting the mutual switching of the A-state exchange columns 100 and the B-state exchange columns 100, each exchange column 100 is connected with the adjusting mechanism 300, and the adjusting mechanism 300 is used for adjusting the shaking and/or the swaying of the exchange columns 100.
The support assembly comprises an A assembly 210 and a B assembly 220, the A assembly 210 comprises two hoop frames and an A rectangular rod group, the two hoop frames are fixedly arranged at two ends of the exchange column 100, the A rectangular rod group comprises two parallel A1 rods 211 and two parallel A2 rods 212, the two A1 rods 211 and the two A2 rods 212 are enclosed to form a rectangle, the A1 rods 211 are arranged along the length direction of the exchange column 100, the two A2 rods 212 are respectively arranged at two ends of the A1 rods 211, the ends of the A1 rods 211 and the ends of the A2 rods 212 are hinged through an A hinge shaft 213, the A hinge shaft 213 is perpendicular to the plane where the A1 rods 211 and the A2 rods 212 are located, the two A2 rods 212 are fixedly connected with the two hoop frames respectively, the adjusting mechanism 300 comprises an A adjusting assembly 310 and a B adjusting assembly 320, the A adjusting assembly 310 is connected with the A1 rods 211 close to the exchange column 100, and the A1 rods 211 close to the exchange column 100 are used for adjusting the reciprocating movement of the A1 rods 211 along the length direction of the other A1 rods 211.
The B assembly 220 includes two sets of B rectangular bar sets disposed at two ends far from the A1 bar 211, the B rectangular bar sets including two parallel B1 bars 221 and two parallel B2 bars 222, the two B1 bars 221 and the two B2 bars 222 enclosing a rectangle, the planes of the two B1 bars 221 and the B2 bars 222 being perpendicular to the A1 bar 211, the ends of the B1 bars 221 and the B2 bars 222 being hinged by a B hinge 223, the B1 bars 221 and the A1 bars 211 being vertically distributed, the two B2 bars 222 being spaced apart along the radial direction of the exchange column 100, one of the B1 bars 221 being denoted as a support bar, one end of the support bar being elongated and being rotatably connected to the a hinge 213, the B2 bar 222 far from the exchange column 100 being connected to the B adjustment assembly 320, the B adjustment assembly 320 being adapted to adjust the rotation of the B2 bars 222 about the B hinge 223.
The B adjusting component 320 comprises a supporting cylinder 321 and a transmission shaft 330, the supporting cylinder 321 is arranged along the length direction of the rod of the A1 rod 211, two B2 rods 222 are fixedly connected with a rotating shaft 322, the axial direction of the rotating shaft 322 is consistent with the length direction of the rod of the A1 rod 211, the two rotating shafts 322 are rotatably arranged at two ends of the supporting cylinder 321, the transmission shaft 330 and the B1 rod 221 are distributed in parallel, one end of the transmission shaft 330 is rotatably arranged in the supporting cylinder 321, and one rotating shaft 322 is connected with the transmission shaft 330 through the B transmission component and the selection component 340.
The A adjusting component 310 comprises a swing arm, the middle part of the swing arm 311 is rotatably mounted on an A1 rod 211 far away from the exchange column through a first hinge shaft 313, a cylindrical pin 312 is fixedly mounted on the A1 rod 211 close to the exchange column 100, the axial directions of the first hinge shaft 313 and the cylindrical pin 312 are consistent, the axial direction of the first hinge shaft 313 is perpendicular to the rod length direction of the A1 rod 211, a guide groove is formed in the swing arm 311 along the arm length direction, the cylindrical pin 312 is slidably mounted in the guide groove, and the other end of the swing arm 311 is connected with a transmission shaft 330 through an A transmission component and a selection component 340.
The A transmission assembly comprises a first supporting rod 314 and a second supporting rod 315, one end of the first supporting rod 314 is hinged to one end of a swing arm 311 away from a cylindrical pin 312 through a second hinge shaft, the other end of the first supporting rod 314 is hinged to one end of the second supporting rod 315 through a third hinge shaft, the axial direction of the second hinge shaft is consistent with the rod length direction of an A1 rod 211, the other end of the second supporting rod 315 is connected with an arc tooth 316, the circle center of the arc tooth 316 is located on the axis of the first hinge shaft 313, the arc tooth 316 is meshed with a rack 318, the rack 318 is arranged along the cylinder length direction of a supporting cylinder 310, the rack 318 is slidably mounted on the outer wall of the supporting cylinder 310 along the length direction of the rack, a constraint assembly is mounted on the outer wall of the supporting cylinder 310 and corresponds to the arc tooth 316, the constraint assembly is used for constraining the arc tooth 316 to move along the thickness direction of the arc tooth 316, and the rack 318 is connected with the selection assembly 340 through the linkage assembly 350.
The restraint subassembly includes two baffles 319, and two baffles 319 and arc tooth 316 both sides sliding fit all offer the arc wall on two baffles 319, and the centre of a circle of arc wall is located the axis of first articulated shaft 313, and arc tooth 316 both sides set up slide pin 317, slide pin 317 slidable mounting is in the arc wall.
The linkage assembly 350 is arranged in the support cylinder 321, the linkage assembly 350 comprises a sliding block 354 and a linkage shaft 351, the linkage shaft 351 and a transmission shaft 330 are arranged along the extension direction, the shaft body of the linkage shaft 351 is rotatably arranged in the support cylinder 321, the sliding block 354 is fixedly connected with a rack 318, a sliding groove is formed in the sliding block 354, the groove direction of the sliding groove is perpendicular to the length direction of the rack 318, one end, close to the sliding block 354, of the linkage shaft 351 is fixedly connected with one end of a linkage arm 352, the linkage arm 352 and the linkage shaft 351 are vertically distributed, one end, far away from the linkage shaft 351, of the linkage arm 352 is provided with a pin 353, and the pin 353 is slidably arranged in the sliding groove.
The B transmission assembly comprises a hollow shaft 325, the hollow shaft 325 is sleeved on a transmission shaft 330, an A bevel gear 324 is arranged on the hollow shaft 325, a B bevel gear 323 is arranged at the end part of the rotating shaft 322, and the A bevel gear 324 is meshed with the B bevel gear 323.
The selection assembly 340 includes two sliding shafts 341, the two sliding shafts 341 are sleeved on the transmission shaft 330, the two sliding shafts 341 form sliding guiding fit with the transmission shaft 330 along the axial direction of the transmission shaft 330, two ends of the two sliding shafts 341 respectively correspond to the ends of the hollow shaft 325 and the linkage shaft 351, the corresponding ends of the two sliding shafts 341, the hollow shaft 325 and the linkage shaft 351 are in a saw-tooth structure, the two sliding shafts 341 are connected with a selection unit, and the selection unit is used for adjusting the two sliding shafts 341 to slide along the axial direction of the transmission shaft 330 so as to be jointed with the hollow shaft 325 and/or the linkage shaft 351.
The end parts of the two sliding shafts 341, which are close to each other, are provided with annular plates 342, the surfaces of the two annular plates 342, which are close to each other, are inclined surfaces, the selection unit comprises a first shifting rod 343, a separation fork rod 345 and a second shifting rod 344, the first shifting rod 343 and the second shifting rod 344 are respectively abutted against the surfaces of the two annular plates 342, which are away from each other, the separation fork rod 345 points to a position between the two annular plates 342, the end parts of the separation fork rod 345 are wedge blocks, the first shifting rod 343 and the second shifting rod 344 are respectively connected with corresponding reciprocating components, the reciprocating components are used for adjusting the first shifting rod 343 or the second shifting rod 344 to move along the axial direction of the transmission shaft 330, the separation fork rod 345 is connected with a telescopic component, and the telescopic component is used for adjusting the telescopic motion of the separation fork rod 345; wherein, the reciprocating component and the telescopic component are all air cylinders, and the movement of the first deflector rod 343 and the second deflector rod 344 is pneumatically adjusted, and the telescopic movement of the separation fork rod 345 is adjusted.
The end of the transmission shaft 330 far away from the exchange column 100 is provided with a C-shaped bevel gear 331, and the upright post 500 is rotatably provided with a bevel gear disk 360, and each C-shaped bevel gear 331 is meshed with the bevel gear disk 360.
The switching mechanism 400 comprises a limiting block 410, a limiting sleeve shaft 420 and a switching unit, wherein the limiting block 410 is fixedly installed, the limiting sleeve shaft 420 is sleeved on a transmission shaft 330, one end of the limiting sleeve shaft 420 is fixedly connected with a supporting cylinder 321, a passive rod 430 is installed at one end of the limiting sleeve shaft 420, which is far away from the supporting cylinder 321, the limiting sleeve shaft 420 is inserted into the limiting block 410, a strip-shaped protrusion is arranged on the outer wall of the limiting sleeve shaft 420, and a groove matched with the limiting block 410 is formed in the limiting block;
the switching unit is correspondingly arranged with each passive rod 430, and is used for abutting against the passive rods 430 to drive the limiting sleeve shafts 420 to extend out of the limiting blocks 410, and after the protrusions are separated from the grooves, the switching unit toggles the passive rods 430, and the passive rods 430 drive the limiting sleeve shafts 420 to rotate ninety degrees, so that the A-state exchange column 100 is switched into the B-state exchange column 100; similarly, the switching unit toggles the passive rod 430 to reset, and then adjusts the passive rod 430 to retract to drive the limiting sleeve shaft 420 to return to the original position, so that the switching of the B-state exchange column 100 into the A-state exchange column 100 is realized.
The use process of the electronic grade hydrochloric acid purifying device provided in the embodiment is as follows:
firstly, 12 groups of exchange columns 100 are arranged in the hydrochloric acid adsorption mechanism 2 in this embodiment, 6 groups of A-state exchange columns 100 are arranged, 6 groups of B-state exchange columns 100 are arranged, hydrochloric acid connectors in each A-state exchange column 100 are connected in series by adopting acid-resistant pipes, hydrochloric acid is introduced into a first A-state exchange column by the hydrochloric acid feeding mechanism 1, the hydrochloric acid is adsorbed by resin in the exchange columns, metal ions such as iron ions are adsorbed, and different motion states of each exchange column 100 can be selected by virtue of selection of pneumatic adjustment, and the specific adjustment process is as follows:
the cylinder adjusts the first deflector rod 343 and the second deflector rod 344 to synchronously move so as to realize the shifting of the sliding shaft 341 between the hollow shaft 325 and the linkage shaft 351, and the transmission shaft 330 idles at this time, so that the exchange column 100 is in a static state;
the cylinder adjusts the first deflector 343 and the second deflector 344 to move synchronously, so as to realize that the sliding shaft 341 is moved to be engaged with the linkage shaft 351, at this time, the transmission shaft 330 drives the linkage shaft 351 to rotate through the sliding shaft 341, the linkage shaft 351 drives the linkage arm 352 to rotate, the linkage arm 352 drives the pin 353 to rotate around the linkage shaft 351, the pin 353 slides back and forth in the sliding groove and drives the sliding block 354 to move up and down, the sliding block 354 drives the rack 318 to move up and down synchronously, the rack 318 is meshed with the arc-shaped tooth 316, the arc-shaped tooth 316 is driven to rotate, the arc-shaped tooth 316 drives the swing arm 311 to swing up and down around the first hinge shaft 313 through the second supporting rod 315 and the first supporting rod 314, the swing arm 311 drives the cylindrical pin 312 to slide in the guide groove in the swing arm 312 and drive the cylindrical pin 312 to move up and down, and the cylindrical pin 312 drives the A1 rod 211 to reciprocate along the rod length direction, so as to drive the exchange column 100 to swing back and forth along the length direction;
the cylinder adjusts the first deflector 343 and the second deflector 344 to move synchronously, so as to achieve the purpose of pulling the sliding shaft 341 into engagement with the hollow shaft 325, at this time, the transmission shaft 330 drives the hollow shaft 325 to rotate through the sliding shaft 341, the hollow shaft 325 drives the A bevel gear 324 to rotate, the A bevel gear 324 drives the B bevel gear 323 to rotate, the B bevel gear 323 drives the rotating shaft 322 to rotate, the rotating shaft 322 drives the B2 rod 222 to rotate, the B2 rod 222 drives the B1 rod 221 to do circular motion around the rotating shaft 322, the B2 rod 222 drives the exchange column to do circular motion in a plane through the A2 rod 212, and the purpose of achieving shaking is achieved through the hinging of the first support rod 314 and the second support rod 315.
The cylinder adjusting and separating fork rod 345 extends, the wedge blocks are inserted into the inclined planes between the two annular plates 342, the two annular plates 342 are driven to separate, the two sliding shafts 341 are adjusted to separate, the two sliding shafts 341 are respectively connected with the hollow shaft 325 and the linkage shaft 351, and the adjusting and exchanging column 100 can shake back and forth and rock.
When hydrochloric acid adsorption treatment is carried out, the first A-state exchange column 100 is adjusted to shake up and down and shake, the second A-state exchange column is adjusted to shake up and down, the third A-state exchange column 100 is adjusted to shake up and down, three A-state exchange columns 100 are left to be static, hydrochloric acid sequentially flows into the six groups of A-state exchange columns 100, high-flow hydrochloric acid can shake and shake resin firstly to carry out rapid mixed contact, first-stage adsorption treatment is achieved, then hydrochloric acid sequentially flows into the two groups of A-state exchange columns 100 with descending resin movement, second-stage and third-stage treatment is achieved, and finally, three groups of static A-state exchange columns 100 sequentially flow into, and static and thorough adsorption is achieved. Through the adsorption step, the aim of rapid adsorption treatment of the large-flow hydrochloric acid is fulfilled.
After each a-state column 100 is operated for a predetermined time, each B-state column 100 is switched to each a-state column 100, and hydrochloric acid is sequentially introduced into each a-state column 100 in the same manner as described above.
Deionized water is introduced into each B-state exchange column 100, and the resin is subjected to elution reduction treatment; the specific process is as follows:
firstly, the B-state exchange column 100 is adjusted to shake and rock, deionized water is continuously introduced, the water flow is rapid at this time, so that the resin and the deionized water are in rapid mixing contact, then, the B-state exchange column 100 is adjusted to be static, the deionized water is continuously introduced, the water flow is slow, thorough elution is realized, and the resin is ready for reuse.
Example 2
In this embodiment, a purification process of electronic grade hydrochloric acid is provided, which includes the following steps:
s1: preparing two groups of exchange columns, namely a group A and a group B, wherein each exchange column in the group A is vertically distributed, each exchange column in the group B is horizontally distributed, and the group A and the group B can be mutually switched;
s2: each exchange column in the group A is sequentially divided into two groups, each exchange column in the front group has decreasing motion freedom degree and amplitude, each exchange column in the rear group is vertically stationary, and then hydrochloric acid is introduced into each exchange column in each group A one by one;
s3: after hydrochloric acid is introduced into the A group exchange column for a preset time, the A group is switched into the B group, the B group is switched into the A group, and hydrochloric acid is introduced into the newly switched A group exchange column;
s4: and (3) eluting and reducing the resin in the group B exchange column.
The embodiment has been described above with reference to the embodiment, but the embodiment is not limited to the above-described specific implementation, which is only illustrative and not restrictive, and many forms can be made by those of ordinary skill in the art, given the benefit of this disclosure, are within the scope of this embodiment.
Claims (8)
1. The purifying device of the electronic grade hydrochloric acid is characterized by comprising a hydrochloric acid feeding mechanism, a hydrochloric acid adsorption mechanism and a hydrochloric acid rectifying mechanism which are sequentially arranged;
the hydrochloric acid adsorption mechanism comprises exchange columns and flushing components, wherein the exchange columns are distributed in a circumferential array around the upright columns, the upright columns are arranged vertically, adsorption resin is filled in each exchange column, two ends of each exchange column are provided with pipe joints, the two pipe joints are connected with the flushing components through water pipes, hydrochloric acid connectors are arranged on the column bodies of the exchange columns, one hydrochloric acid connector is connected with the hydrochloric acid feeding mechanism, and the other hydrochloric acid connector is connected with the hydrochloric acid rectifying mechanism;
each exchange column is arranged on a supporting mechanism, and the supporting mechanism comprises supporting components which are arranged in a one-to-one correspondence manner; the support component is connected with the switching mechanism, each exchange column is connected with the adjusting mechanism, and the adjusting mechanism is used for adjusting the shaking and/or the swaying of the exchange column;
the support assembly comprises an A assembly and a B assembly, the A assembly comprises two hoop frames and an A rectangular rod group, the two hoop frames are fixedly arranged at two ends of the exchange column, the A rectangular rod group comprises two parallel A1 rods and two parallel A2 rods, the two A1 rods and the two A2 rods form a rectangle, the A1 rods are arranged along the length direction of the exchange column, the two A2 rods are respectively arranged at two ends of the A1 rods, the ends of the A1 rods and the ends of the A2 rods are hinged through A hinge shafts, the A hinge shafts are perpendicular to planes of the A1 rods and the A2 rods, the two A2 rods are fixedly connected with the two hoop frames respectively, the A adjusting mechanism comprises an A adjusting assembly and a B adjusting assembly, the A adjusting assembly is connected with the A1 rods close to the exchange column, and the A adjusting assembly is used for adjusting the A1 rods close to the exchange column to reciprocate along the length direction of the other A1 rods;
the B component comprises two groups of B rectangular rod groups, the two groups of B rectangular rod groups are arranged at two ends far away from the A1 rod, the B rectangular rod groups comprise two parallel-distributed B1 rods and two parallel-distributed B2 rods, the two B1 rods and the two B2 rods enclose a rectangle, the plane where the two B1 rods and the B2 rods are located is perpendicular to the A1 rod, the end parts of the B1 rods and the B2 rods are hinged through a B hinge shaft, the B1 rods and the A1 rods are vertically distributed, the two B2 rods are radially distributed at intervals along the exchange column, one B1 rod is recorded as a supporting rod, one end of the supporting rod is prolonged and is rotationally connected with the A hinge shaft, the B2 rod far away from the exchange column is connected with a B adjusting component, and the B adjusting component is used for adjusting the rotation of the B2 rod around the B hinge shaft.
2. The purifying device for electronic grade hydrochloric acid according to claim 1, wherein the B adjusting assembly comprises a supporting cylinder and a transmission shaft, the supporting cylinder is arranged along the length direction of the A1 rod, the two B2 rods are fixedly connected with the rotating shaft, the axial direction of the rotating shaft is consistent with the length direction of the A1 rod, the two rotating shafts are rotatably arranged at two ends of the supporting cylinder, the transmission shaft and the B1 rod are distributed in parallel, one end of the transmission shaft is rotatably arranged in the supporting cylinder, and one rotating shaft is connected with the transmission shaft through the B transmission assembly and the selection assembly.
3. The purification device of electronic grade hydrochloric acid according to claim 2, wherein the a adjusting component comprises a swing arm, the middle part of the swing arm is rotatably installed on an A1 rod far away from the exchange column through a first hinge shaft, a cylindrical pin is fixedly installed on the A1 rod close to the exchange column, the first hinge shaft is consistent with the axial direction of the cylindrical pin, the axial direction of the first hinge shaft is perpendicular to the length direction of the rod of the A1 rod, a guide groove is formed in the swing arm along the length direction of the arm, the cylindrical pin is slidably installed in the guide groove, and the other end of the swing arm is connected with a transmission shaft through an a transmission component and a selection component.
4. The purification device of electronic grade hydrochloric acid according to claim 3, wherein the A transmission component comprises a first supporting rod and a second supporting rod, one end of the first supporting rod is hinged with one end of a swing arm far away from a cylindrical pin through a second hinge shaft, the other end of the first supporting rod is hinged with one end of the second supporting rod through a third hinge shaft, the second hinge shaft is consistent with the axial direction of the third hinge shaft, the axial direction of the second hinge shaft is consistent with the rod length direction of the A1 rod, the other end of the second supporting rod is connected with an arc-shaped tooth, the center of the arc-shaped tooth is positioned on the axis of the first hinge shaft, the arc-shaped tooth is meshed with a rack, the rack is arranged along the length direction of a supporting cylinder, the rack is slidably mounted on the outer wall of the supporting cylinder along the length direction of the supporting cylinder, the constraint component is arranged corresponding to the arc-shaped tooth, and the constraint component is used for constraining the arc-shaped tooth to move along the thickness direction of the arc-shaped tooth and is connected with the selection component through the linkage component.
5. The purification device of electronic grade hydrochloric acid according to claim 4, wherein the linkage assembly is arranged in the supporting cylinder, the linkage assembly comprises a sliding block and a linkage shaft, the linkage shaft and the transmission shaft are arranged along the extension direction, the shaft body of the linkage shaft is rotatably arranged in the supporting cylinder, the sliding block is fixedly connected with the rack, a sliding groove is formed in the sliding block, the groove direction of the sliding groove is perpendicular to the length direction of the rack, one end, close to the sliding block, of the linkage shaft is fixedly connected with one end of the linkage arm, the linkage arm and the linkage shaft are vertically distributed, a pin shaft is arranged at one end, far away from the linkage shaft, of the linkage arm, and the pin shaft is slidably arranged in the sliding groove.
6. The purification device of electronic grade hydrochloric acid according to claim 5, wherein the B transmission assembly comprises a hollow shaft, the hollow shaft is sleeved on the transmission shaft, an a bevel gear is mounted on the hollow shaft, a B bevel gear is mounted at the end of the rotation shaft, and the a bevel gear is meshed with the B bevel gear.
7. The purification device of electronic grade hydrochloric acid according to claim 6, wherein the selection component comprises two sliding shafts, the two sliding shafts are sleeved on the transmission shaft, the two sliding shafts and the transmission shaft form sliding guide fit along the axial direction of the transmission shaft, two ends of the two sliding shafts respectively correspond to the end parts of the hollow shaft and the linkage shaft, the corresponding end parts of the two sliding shafts, the hollow shaft and the linkage shaft are of a saw-tooth structure, the two sliding shafts are connected with the selection unit, and the selection unit is used for adjusting the two sliding shafts to slide along the axial direction of the transmission shaft so as to realize the joint with the hollow shaft and/or the linkage shaft.
8. An electronic grade hydrochloric acid purification process using the purification apparatus of electronic grade hydrochloric acid as set forth in claim 1, characterized by comprising the steps of:
s1: preparing two groups of exchange columns, namely a group A and a group B, wherein each exchange column in the group A is vertically distributed, each exchange column in the group B is horizontally distributed, and the group A and the group B can be mutually switched;
s2: each exchange column in the group A is sequentially divided into two groups, each exchange column in the front group has decreasing motion freedom degree and amplitude, each exchange column in the rear group is vertically stationary, and then hydrochloric acid is introduced into each exchange column in each group A one by one;
s3: after hydrochloric acid is introduced into the A group exchange column for a preset time, the A group is switched into the B group, the B group is switched into the A group, and hydrochloric acid is introduced into the newly switched A group exchange column;
s4: and (3) eluting and reducing the resin in the group B exchange column.
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| US4952386A (en) * | 1988-05-20 | 1990-08-28 | Athens Corporation | Method and apparatus for purifying hydrogen fluoride |
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| CN205506774U (en) * | 2016-03-01 | 2016-08-24 | 中国石油化工股份有限公司 | Duolite device of survey sulfonic acid group content |
| CN110371933A (en) * | 2019-07-27 | 2019-10-25 | 哈尔滨师范大学 | A kind of method of purification of spent acid |
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| US4952386A (en) * | 1988-05-20 | 1990-08-28 | Athens Corporation | Method and apparatus for purifying hydrogen fluoride |
| CN1292023A (en) * | 1998-03-02 | 2001-04-18 | 密执安生物技术所 | Purification of organic acid using anion exchange chromatography |
| CN1704398A (en) * | 2004-05-26 | 2005-12-07 | 中国科学院过程工程研究所 | Method for one-step purification and separation of ephedrine by cation exchange resin and expanded bed integrated technology |
| CN205506774U (en) * | 2016-03-01 | 2016-08-24 | 中国石油化工股份有限公司 | Duolite device of survey sulfonic acid group content |
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Address after: 215300 No.66 Wenpu Middle Road, Qiandeng Town, Kunshan City, Suzhou City, Jiangsu Province Patentee after: Lianshi New Materials (Suzhou) Co.,Ltd. Address before: 215300 No.66 Wenpu Middle Road, Qiandeng Town, Kunshan City, Suzhou City, Jiangsu Province Patentee before: Lianshi (Kunshan) chemical materials Co.,Ltd. |