CN218307855U - Small-size perfluoro ion exchange membrane reactor for hydrolytic transformation - Google Patents
Small-size perfluoro ion exchange membrane reactor for hydrolytic transformation Download PDFInfo
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- CN218307855U CN218307855U CN202221860625.1U CN202221860625U CN218307855U CN 218307855 U CN218307855 U CN 218307855U CN 202221860625 U CN202221860625 U CN 202221860625U CN 218307855 U CN218307855 U CN 218307855U
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- 239000003014 ion exchange membrane Substances 0.000 title claims abstract description 107
- 230000009466 transformation Effects 0.000 title claims abstract description 45
- -1 perfluoro Chemical group 0.000 title claims abstract description 14
- 230000003301 hydrolyzing effect Effects 0.000 title description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 90
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 78
- 230000007062 hydrolysis Effects 0.000 claims abstract description 68
- 238000005485 electric heating Methods 0.000 claims description 18
- 239000000413 hydrolysate Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 abstract description 18
- 238000011160 research Methods 0.000 abstract description 11
- 239000012528 membrane Substances 0.000 description 26
- 229910001220 stainless steel Inorganic materials 0.000 description 15
- 239000010935 stainless steel Substances 0.000 description 15
- 238000004519 manufacturing process Methods 0.000 description 14
- 238000002474 experimental method Methods 0.000 description 11
- 239000003513 alkali Substances 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000002585 base Substances 0.000 description 7
- 238000013461 design Methods 0.000 description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000005342 ion exchange Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229910000619 316 stainless steel Inorganic materials 0.000 description 5
- 238000010924 continuous production Methods 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000005457 optimization Methods 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000011020 pilot scale process Methods 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ABDBNWQRPYOPDF-UHFFFAOYSA-N carbonofluoridic acid Chemical compound OC(F)=O ABDBNWQRPYOPDF-UHFFFAOYSA-N 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012803 optimization experiment Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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Abstract
The utility model belongs to the technical field of ion exchange membrane, concretely relates to small-size perfluoro ion exchange membrane reactor for transformation of hydrolysising. The small reactor for the hydrolysis transformation of the perfluorinated ion exchange membrane comprises a reaction tank, a circulating pump, an ion exchange membrane hanger and a placing rack matched with the inner size of the reaction tank; the ion exchange membrane hanger comprises a spring, a needle plate, an outer frame matched with the size of the placement frame and a needle plate fixing plate arranged in the outer frame. The hydrolysis reactor can complete the hydrolysis reaction of the perfluorinated ion exchange membrane with a specific size, especially a small size, and can be applied to the research process of the hydrolysis reaction parameters of the perfluorinated ion exchange membrane in a laboratory environment.
Description
Technical Field
The utility model belongs to the technical field of ion exchange membrane, concretely relates to small-size perfluoro ion exchange membrane reactor for transformation of hydrolysising.
Background
The perfluorinated ion exchange membrane (chlor-alkali ion membrane) is a perfluorocarboxylic acid-perfluorosulfonic acid composite membrane, namely, the anode side of the membrane is a perfluorosulfonic acid layer, and the cathode side of the membrane is a perfluorocarboxylic acid layer. During the processing of the perfluorinated ion exchange membrane, the precursor does not have ion exchange capacity. In order to obtain ion exchange capacity, the precursor needs to undergo a hydrolytic transformation process in alkaline solution, with-SO 2 F and-COOCH 3 The radicals being converted separately into-SO having ion-exchange capacity 3 - M + and-COO - M + A group. Therefore, the hydrolysis transformation reaction of the perfluorinated ion exchange membrane is the most critical process step of the ion exchange membrane with the ion exchange function.
In the continuous production process of the existing perfluorinated ion exchange membrane, a hydrolysis transformation process generally needs larger equipment as a support, and the hydrolysis transformation process is carried out on various tension frames, treatment tanks and guide rollers in a membrane roll form. Usually, a roll has three to four hundred meters and the width is 1400 to 2000mm, the continuous production is many hundreds of meters, and the raw material solution is consumed by one time of starting the machine for at least tens of kilograms. Although the large-scale perfluorinated ion exchange membrane hydrolysis reaction equipment is suitable for large-scale industrial production, the large-scale perfluorinated ion exchange membrane hydrolysis reaction equipment is not suitable for the situations of small-scale perfluorinated ion exchange membrane hydrolysis transformation reactions such as experimental research, pilot-scale experiments and the like.
Taking experimental research as an example, when technicians need to optimize and design hydrolysis transformation process parameters of the perfluorinated ion exchange membrane, the size of a perfluorinated ion exchange membrane sample required in the experimental research process is small, and the membrane specification can be as small as 5 multiplied by 20mm; and the membrane needs to be treated piece by piece, being discontinuous. Meanwhile, the required experimental solvents and the like are less in dosage, but the existing large-scale equipment is obviously not suitable, so that the operation is inconvenient, and the waste of raw materials is caused.
Therefore, a small-scale reactor for hydrolysis conversion of perfluorinated ion exchange membranes is needed to adapt to small-scale hydrolysis reaction of ion exchange membranes.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a small-size perfluoro ion exchange membrane reactor for transformation of hydrolysising through this hydrolysis reactor, can accomplish specific size, especially small-size perfluoro ion exchange membrane's hydrolysis, especially can be applied to the research in-process to perfluoro ion exchange membrane hydrolysis parameters under the laboratory environment.
The technical scheme of the utility model is that: a small reactor for the hydrolysis transformation of a perfluorinated ion exchange membrane comprises a reaction tank, a circulating pump, an ion exchange membrane hanger and a placing rack matched with the inner size of the reaction tank; a heating device, a temperature measuring device and a hydrolysate circulating pipeline are arranged in the reaction tank, wherein the hydrolysate circulating pipeline is connected with a circulating pump; the placing frame is independent of the reaction tank; limiting grooves for fixing the ion exchange membrane hanging rack are symmetrically arranged on two sides in the placing rack; the ion exchange membrane hanger comprises a spring, a needle plate, an outer frame matched with the size of the placing frame and a needle plate fixing plate arranged in the outer frame; a positioning plate is arranged on the outer side of the outer frame and corresponds to the limiting groove of the placing frame; spring fixing holes are formed in four edges of the outer frame; the number of the needle plate fixing plates is 4, a spring fixing hole is arranged on one long edge of each needle plate fixing plate, and when the needle plate fixing plate is used, the needle plate fixing plates are connected with the outer frame through the springs and the spring fixing holes; a needle plate fixing hole for fixing the needle plate is arranged on the other long edge of each needle plate fixing plate; two short side ends of each needle plate fixing plate are respectively provided with a connecting hole for fixedly connecting 4 needle plate fixing plates; the needle plate comprises a needle and a base, wherein the base of the needle plate is provided with a needle plate fixing hole, and the needle plate fixing hole corresponds to the needle plate fixing hole arranged on the needle plate fixing plate.
Further, the rotating speed of a circulating pump in the reactor for hydrolysis transformation of the small perfluorinated ion exchange membrane is 2750-3150 rpm, the flow rate is 13-15L/min, the power is 70-90W, and the rated voltage is 220V; the heating device is an electric heating pipe; the temperature measuring device is a thermocouple. The indexes of the rotating speed, the flow, the power and the rated voltage of the circulating pump are specially designed according to the characteristics of the perfluorinated ion exchange membrane, and the circulating pump under the indexes can simulate the liquid circulating impact force of large-scale equipment on the perfluorinated ion exchange membrane in actual continuous production, thereby laying a foundation for the scientificity and the practicability of the hydrolysis transformation reaction optimization experiment of the ion exchange membrane.
Furthermore, the electric heating tube in the small reactor for the hydrolysis transformation of the perfluorinated ion exchange membrane extends downwards to the bottom of the reaction tank along the inner wall of the narrow side of the reaction tank and is uniformly laid at the bottom of the reaction tank, so that the hydrolysis reaction liquid is uniformly heated; the distance between the electric heating pipe and the inner wall of the narrow side is less than or equal to 50mm, and through the design, the solution can be efficiently heated, and the volume occupied in the reaction tank is less; the number of the thermocouples is at least 1, and the thermocouples are arranged at the position which is less than or equal to 1000mm away from the bottom of the reaction tank. The design ensures that the volume occupied in the reaction tank is reduced as much as possible, simultaneously ensures that the real temperature of the hydrolysis solution in the reaction tank is accurately measured, and avoids the measurement data from being influenced by the metal heat conduction of the reaction tank. After all, if the method is used for researching and optimizing hydrolysis transformation process parameters, the accuracy of data measurement is very important for researching scientific reliability.
Further, a liquid inlet of a hydrolysate circulating pipeline in the small perfluorinated ion exchange membrane hydrolysis conversion reactor is fixed at a position which is less than or equal to 200mm away from the top of the reaction tank; the liquid outlet is fixed at a position which is less than or equal to 200mm away from the bottom of the reaction tank.
Further, the internal dimension height of the reaction tank in the reactor for hydrolysis conversion of the small-sized perfluorinated ion exchange membrane is as follows: length: the width is 1-10. The size proportion is designed according to the actual requirements of hydrolysis transformation reaction, completely meets the hydrolysis reaction of the perfluorinated ion exchange membranes with various specific sizes, and is completely suitable for the research of the hydrolysis reaction parameters of the perfluorinated ion exchange membranes in a laboratory.
Furthermore, the two sides of a limiting groove in the small reactor for the hydrolysis transformation of the perfluorinated ion exchange membrane are symmetrically arranged into a group; each group of adjacent limiting grooves are equidistant; a limiting plate is arranged in the limiting groove.
Furthermore, a handle is arranged above a placing frame in the reactor for hydrolysis and transformation of the small perfluorinated ion exchange membrane, so that the placing frame can be conveniently placed in the reaction tank.
Further, the outer frame in the small-sized reactor for the hydrolysis transformation of the perfluorinated ion exchange membrane is square.
Furthermore, the tension range of the spring in the small reactor for the hydrolysis transformation of the perfluorinated ion exchange membrane is 0.1-100N.
Further, the length of the needle in the small reactor for the hydrolysis transformation of the perfluorinated ion exchange membrane is 2-20 mm; the needles are distributed on the base in 1-3 rows, and the included angle between the needles and the needle plate fixing plate is more than or equal to 45 degrees and less than 90 degrees. Considering that the ion membrane is swelled and enlarged in size in the process of hydrolysis transformation reaction of the perfluorinated ion exchange membrane, an included angle between a needle in a needle plate for fixing the perfluorinated ion exchange membrane and a needle plate fixing plate is designed to be more than or equal to 45 degrees and less than 90 degrees; if the concentration is not within the range, such as a right angle or an obtuse angle is formed between the needle and the needle plate fixing plate, the ion exchange membrane is easy to fall off in the reaction process; however, if the included angle between the needle and the needle plate fixing plate is too small, the membrane body is difficult to pass through the needle when the ion exchange membrane is fixed, the operation difficulty is increased, but the membrane is easy to cause artificial loss, some unknown influence factors are brought, and the inaccuracy of research parameters can be caused if the membrane is used for an optimization design experiment.
The beneficial effects of the utility model are that: the utility model discloses a small-size perfluoro ion exchange membrane hydrolysis transformation is the discontinuous formula with the reactor, can be with the processing perfluoro ion exchange membrane of a slice, and the minimum specification that ion exchange membrane that this reaction unit can handle can reach 5 x 20mm, is applicable to various small-scale perfluoro ion exchange membrane hydrolysis transformation reactions, and the scope is extensive.
The small-sized reactor for the hydrolysis transformation of the perfluorinated ion exchange membrane comprises a reaction tank, a circulating pump, an ion exchange membrane hanging rack and a placing rack matched with the inner size of the reaction tank. The ion exchange membrane hanger comprises a spring, a needle plate, an outer frame matched with the size of the placement frame, and a needle plate fixing plate arranged in the outer frame.
In combination with the above design, the basic principle of the reactor is as follows: fixing the perfluorinated ion exchange membrane on the needle plate fixing plate by using a needle on the needle plate, connecting the needle plate fixing plate with an outer frame by using a spring, and removing screws which are used for connecting and fixing the needle plate fixing plate in the horizontal direction and the vertical direction, so that the needle plate fixing plate drives the needle plate, and further drives the perfluorinated ion exchange membrane to bear the tension of the spring, wherein the tension is the same as the tension of equipment on the membrane in the actual production process, and the tension can be adjusted by adjusting the type of the spring; fixing the ion exchange membrane rack with the membrane on a placing rack, integrally placing the ion exchange membrane rack with the membrane into a reaction tank filled with a constant-temperature solution, and starting a circulating pump. Thus, the small-scale hydrolysis process of the perfluorinated ion exchange membrane can be completed.
The membrane can be subjected to tension through the linkage relation among the parts, particularly, the design of the spring is more flexible, and if the reactor is used for an optimization design experiment, the tension caused by large-scale equipment of different models in actual production can be simulated, so that the research result is more suitable for actual production and is more scientific and effective.
The small reactor for the hydrolysis transformation of the perfluorinated ion exchange membrane has the advantages that: the hydrolysis reactor has the advantages that the raw material cost is saved, the volume of the hydrolysis reactor can be designed to be very small according to actual requirements due to the structural characteristics of the hydrolysis reactor, the solution raw materials required for reaction and the size specification of the perfluorinated ion exchange membrane can be configured according to the actual requirements, the reaction can be completed in the hydrolysis reactor even if the used solvent is very small and the specification of the ion exchange membrane for reaction is very small, the operation method is simple and easy to implement, and the hydrolysis reactor is suitable for hydrolysis conversion reactions of various small-scale perfluorinated ion exchange membranes, especially hydrolysis conversion reactions in experimental research environments.
Drawings
FIG. 1 is a schematic view of the three-dimensional structure of a small and medium-sized reactor for hydrolysis and transformation of a perfluorinated ion exchange membrane according to an embodiment of the present invention.
FIG. 2 is a top view of a reactor for hydrolysis and transformation of a small and medium-sized perfluorinated ion exchange membrane according to an embodiment of the present invention.
Fig. 3 is a schematic perspective view of a reaction tank in the reactor according to the embodiment of the present invention.
FIG. 4 is a front view of a reaction tank in the reactor according to an embodiment of the present invention.
Fig. 5 is a left side view of a reaction tank in the reactor according to the embodiment of the present invention.
FIG. 6 is a top view of a reaction tank in the reactor according to an embodiment of the present invention.
Fig. 7 is a schematic perspective view of a rack in the reactor according to the embodiment of the present invention.
Fig. 8 is an enlarged view of a portion of the spacing groove of fig. 7.
FIG. 9 is a front view of a shelf in the reactor according to an embodiment of the present invention.
Fig. 10 is a left side view of a shelf in the reactor according to an embodiment of the present invention.
FIG. 11 is a top view of a rack placed in a reactor according to an embodiment of the present invention.
Fig. 12 is a schematic three-dimensional structure diagram of an ion exchange membrane rack in the reactor according to the embodiment of the present invention.
Fig. 13 is a front view of an ion exchange membrane rack in a reactor according to an embodiment of the present invention.
Fig. 14 is a left side view of an ion exchange membrane hanger in a reactor according to an embodiment of the present invention.
Fig. 15 is a top view of an ion exchange membrane hanger in a reactor according to an embodiment of the present invention.
FIG. 16 is a front view of an outer frame in the reactor according to an embodiment of the present invention.
Fig. 17 is a left side view of an outer frame in a reactor according to embodiments of the present invention.
Fig. 18 is a schematic perspective view of a needle plate fixing plate positioned in a vertical direction in the reactor according to an embodiment of the present invention.
Fig. 19 is a front view of a needle plate fixing plate in a vertical direction in the reactor according to the embodiment of the present invention.
Fig. 20 is a schematic perspective view of a horizontal needle plate fixing plate in the reactor according to the embodiment of the present invention.
Fig. 21 is a front view of a horizontal needle plate fixing plate in the reactor according to the embodiment of the present invention.
Fig. 22 is a top view of a horizontally oriented pin plate retaining plate in a reactor according to an embodiment of the present invention.
Wherein, 1 is an electric heating pipe, 2 is a thermocouple, 3 is a hydrolysate circulation pipeline, 4 is a limiting groove, 5 is a limiting plate, 6 is a handle, 7 is an outer frame, 8 is a needle plate fixing plate, 9 is a needle plate, 10 is a positioning plate, 11 is a spring fixing hole, 12 is a needle plate fixing hole, 13 is a connecting hole, and 14 is a placing frame.
Detailed Description
The technical solution of the present invention will be described in detail with reference to the accompanying drawings.
The small reactor for the hydrolysis transformation of the perfluorinated ion exchange membrane comprises a circulating pump, a reaction tank, a placing rack 14 and an ion exchange membrane hanging rack.
The rotating speed of the circulating pump is 2750-3150 rpm, the flow rate is 13-15L/min, the power is 70-90W, and the rated voltage is 220V. The material of circulating pump in the reactor for small-size perfluor ion exchange membrane hydrolysis transformation is PVDF, and the inner cavity of the reactor is coated with PTFE. The circulating pump has the characteristics of acid and alkali resistance and high temperature resistance, so that the circulating pump is suitable for technological parameter research experiments of hydrolysis transformation of a plurality of perfluorinated ion exchange membranes.
The internal dimension height of the reaction tank: length: the width is 1-10; preferably, the reaction vessel has internal dimensions of 200 to 1000mm in height, 200 to 1000mm in length and 100 to 500mm in width. The optimized size range does not cause waste of materials and the like due to overlarge size, and the undersize cannot be suitable for the condition of an ion exchange membrane with a larger size.
An electric heating pipe 1, a thermocouple 2 and a hydrolysate circulating pipeline 3 are arranged in the reaction tank.
Wherein the electric heating pipe 1 extends downwards to the bottom of the reaction tank along the inner wall of the narrow side of the reaction tank and is uniformly laid on the bottom of the reaction tank. The distance between the electric heating tube 1 and the inner wall of the narrow side is less than or equal to 50mm; the outer diameter of the electric heating tube 1 is 5-20 mm, and the inner diameter is 3-18 mm. The laying route of the electric heating pipe 1 forms the following view in the reaction tank: as shown in fig. 4, the electric heating tube 1 is shaped like an "L" in the reaction tank in front view; as shown in FIG. 5, the electric heating tube 1 is shaped like a "U" in the reaction tank in the left view; as shown in FIG. 6, the electric heating tube 1 is shaped like a "U" in a plan view in the reaction tank. Wherein the distance between the outer walls of the U-shaped heating pipes is less than or equal to 490mm. The pipe wall of the electric heating pipe is connected with the interface of the inner wall of the reaction tank in a welding way and is externally connected with an electric heating control system.
At least 1 thermocouple 2 may be installed in the lower part of the reaction tank and one below the liquid level of the hydrolysis solution. The thermocouple 2 may be installed in a direction parallel to or perpendicular to or at an angle to the bottom of the reaction tank.
The thermocouple 2 is arranged at a position which is less than or equal to 1000mm away from the bottom of the reaction tank; preferably, the thermocouple 2 is arranged at a position 50-800 mm away from the bottom of the reaction tank; more preferably, the thermocouple 2 is installed at a position 80 to 500mm from the bottom of the reaction tank.
A liquid inlet of the hydrolysate circulating pipeline 3 is fixed at a position which is less than or equal to 200mm away from the top of the reaction tank; the liquid outlet is fixed at a position which is less than or equal to 200mm away from the bottom of the reaction tank; the outer diameter of the part of the circulation pipeline in the hydrolysate circulation pipeline 3, which is positioned outside the reaction tank, is 5-20 mm, the inner diameter of the part is 3-18 mm, and the part is connected with a circulation pump through a hose with the outer diameter of 3-18 mm and the inner diameter of 1-16 mm.
The placing frame 14 is independent of the reaction tank and can flexibly place, take and disassemble the frame, and the limiting grooves 4 for fixing the ion exchange membrane hanging frame are symmetrically arranged in two sides of the frame. The two sides of the limiting groove 4 are symmetrically arranged into a group, and the number of the limiting groove is 1-10 in total, and the limiting groove can be used for fixing 1-10 ion exchange membrane hangers; each group of adjacent limiting grooves 4 are equidistant; the groove depth of the limiting groove 4 is 1-15 mm, and the groove width is 1-15 mm; and a limiting plate 5 is arranged in the limiting groove 4 and used for further fixing the position of the ion exchange membrane hanging rack.
The length of the placing rack 14 is 150-850 mm, the width is 50-450 mm, and the height is 150-950 mm; the material is selected from one of 304, 310s, 316 or 316L-grade stainless steel;
the handle 6 is arranged above the placing rack 14, so that the placing rack can be conveniently placed in and taken out of the reaction tank, wherein the height of the handle 6 is 50-200 mm, and the width of the handle 6 is 50-200 mm. The material of the handle 6 can be selected from one of 304, 310s, 316 and 316L stainless steel or stainless steel externally plated with copper and iron.
The ion exchange membrane hanger comprises a spring, a needle plate 9, an outer frame 7 matched with the size of the placing frame 14, and a needle plate fixing plate 8 arranged in the outer frame 7.
The outer frame 7 is square, the width of the outer side of the outer frame 7 is 150-850 mm, the length of the outer side is 150-950 mm, the thickness is 1-50 mm, the width of the inner side of the outer frame 7 is 100-840 mm, and the length of the inner side is 120-920 mm. The material of the outer frame 7 can be selected from one of 304, 310s, 316L stainless steel or stainless steel plated with copper or iron.
A positioning plate 10 is arranged on the outer side of the outer frame 7, the positioning plate 10 corresponds to the limiting groove 4 of the placing rack, the width of the positioning plate 10 is 1-15 mm, and the thickness of the positioning plate 10 is 1-15 mm. Four edges of the outer frame 7 are provided with 1-20 spring fixing holes 11.
4 needle plate fixing plates 8 are provided, and the thickness of each needle plate fixing plate is 1-50 mm; wherein the length of each of the 2 needle plate fixing plates 8 is 115-915 mm, and the 2 needle plate fixing plates 8 within the length range are used as the upper and lower horizontal edges; the total length of the spring fixing holes in the needle plate fixing plate 8 in the horizontal direction is 1 to 875mm.
The lengths of the other 2 needle plate fixing plates 8 are all 95 to 835mm, and the 2 needle plate fixing plates 8 within the length range are used as left and right vertical edges. The total length of the spring fixing holes on the needle plate fixing plate 8 in the vertical direction is 1-795 mm.
The material of the needle plate fixing plate 8 can be selected from one of 304, 310s, 316 and 316L-grade stainless steel or stainless steel externally plated with copper and iron.
One long edge of each needle plate fixing plate 8 is provided with 1-20 spring fixing holes 11, and when in use, the needle plate fixing plates 8 are connected with the outer frame 7 through the springs and the spring fixing holes 11; needle board fixing holes 12 for fixing the needle boards 9 are provided at the other long edge of each needle board fixing board 8.
Two short side ends of each needle board fixing board 8 are respectively provided with a connecting hole 13 for fixedly connecting 4 needle board fixing boards 8. The horizontal and vertical needle plate fixing plates 8 are fixed to each other through the connecting holes 13. When 4 needle board fixing plates are enclosed to form a 'return' shape, the spring fixing holes 11 are arranged on the periphery of the 'return' shape, and the needle board fixing holes 12 are arranged on the inner periphery of the 'return' shape.
As shown in fig. 20 to 22, the needle plate holding plates 8 located in the horizontal direction are formed in a "convex" shape as a whole, and the needle plate holding plates 8 having the middle portions of the spring holding holes 11 are higher than the needle plate holding plates 8 having the connecting holes 13 on both sides by the thickness of one needle plate holding plate.
The aperture of the spring fixing hole 11 is 1-10 mm.
The needle plate 9 for fixing the perfluorinated ion exchange membrane comprises a needle and a base. The length of the base is 20-880 mm, and the width of the base is 5-30 mm; the length of the needle is 2-20 mm; the number of needles contained in each needle plate is 1 to 440; the needles are distributed in 1-3 rows in the length direction of the base. The material of the needle plate can be selected from one of 304, 310s, 316 and 316L stainless steel or stainless steel externally plated with copper and iron.
Wherein the included angle between the needle and the needle plate fixing plate 8 is more than or equal to 45 degrees and less than 90 degrees.
The base of the needle plate 9 is provided with 2 to 10 needle plate fixing holes 12 for fixing the needle plate, and the needle plate fixing holes correspond to the needle plate fixing holes arranged on the needle plate fixing plate.
The tension range of the spring is 0.1-100N. The material of the spring can be selected from one of 304, 310s, 316 and 316L stainless steel.
Example 1
The small reactor A for the hydrolysis transformation of the perfluorinated ion exchange membrane is made of 310s stainless steel, the length of the reaction tank is 480mm, the width of the reaction tank is 250mm, the height of the reaction tank is 450mm, the internal electric heating tubes 1 are distributed on the inner wall of one side of the width direction of the reaction tank and the bottom of the reaction tank in a U shape, the side faces of the reaction tank are integrally L-shaped, the two thermocouples 2 are respectively arranged on the side walls of the width direction 100mm and 390mm away from the bottom of the reaction tank, the direction of the two thermocouples forms an angle of 90 degrees with the side wall of the width direction of the reaction tank, 25 portions of NaOH +10 portions of DMSO (28.5 kg) are arranged in a laboratory, the two thermocouples are added into the reaction tank, the temperature is adjusted to 70 ℃, a circulating pump made of PVDF with PTFE coated in the inner cavity is opened for solution circulation, the rotating speed is 2750rpm, the flow rate is 15L/min, the power is 90W, the rated voltage is 220V, and the constant temperature is kept for half an hour.
Fixing a copper-plated stainless steel needle plate 9 with the length of 190mm and the width of 20mm on a needle plate fixing plate 8 arranged in the horizontal direction through screws, wherein the side length of the needle plate fixing plate 8 in the horizontal direction is 250mm; a copper-plated stainless steel needle plate 9 having a length of 160mm and a width of 20mm was fixed by screws to a needle plate fixing plate 8 placed in a vertical direction, wherein the side of the needle plate fixing plate 8 in the vertical direction was 220mm.
Then the needle plate fixing plates arranged in the horizontal direction and the needle plate fixing plates arranged in the vertical direction are fixed in pairs through screws to form a rectangle.
Cutting a hydrolysis precursor chlor-alkali ion exchange membrane sampled from the continuous production into samples with the length of 200mm and the width of 180mm, 5 pieces in total, fixing the samples on a needle plate, connecting four edges of a needle plate fixing plate 8 to four edges of an outer frame 7 by adopting 10N 316 stainless steel springs, and using two springs for each edge; the screws that fix the horizontal and vertical needle plate fixing plates are removed, so that the membrane is completely under the tension from the springs.
The five groups of outer frames 7 fixed with the membranes are inserted into the placing rack 14 along the limiting groove 4, the length of the placing rack 14 is 400mm, the width of the placing rack is 220mm, the height (without a handle part) of the placing rack is 300mm, the height of the handle 6 is 100mm, and 5 groups of outer frames can be inserted.
Putting the whole placing rack 14 into a hydrolysis reaction tank, covering a stainless steel cover for 310s, reacting for 60min, removing the placing rack 14, taking the hydrolyzed membrane down, and cleaning the surface with water to obtain 5 chlor-alkali ion exchange membranes with ion exchange capacity.
Example 2
The small reactor B for the transformation of perfluoroion exchange membrane by hydrolysis was charged into the reaction vessel with 20% NaOH +5% DMSO 18.3kg in the laboratory and the temperature was adjusted to 70 ℃. The reaction apparatus A was the same as the reaction apparatus A in example 1 except that the reaction apparatus B had a reaction vessel with a length of 480mm, a width of 160mm and a height of 450mm.
The hydrolysis precursor chlor-alkali ion exchange membrane sampled from the continuous production is cut into samples with the length of 200mm and the width of 180mm, and the samples are fixed on a needle plate, wherein the total number of the samples is 3.
The three groups of outer frames fixed with the membranes are inserted into a placing rack along a limiting groove, the length of the placing rack is 400mm, the width of the placing rack is 150mm, the height (without a handle part) of the placing rack is 300mm, the height of the handle is 100mm, and 3 groups of outer frames can be inserted.
Putting the whole placing rack 14 into a hydrolysis reaction tank, covering a stainless steel cover for 310s, reacting for 60min, removing the placing rack, taking the hydrolyzed membrane down, and cleaning the surface with water to obtain 3 chlor-alkali ion exchange membranes with ion exchange capacity.
Experimental example 1
1. Purpose of the experiment: test the precision of the reactor for hydrolysis transformation of the small perfluorinated ion exchange membrane for simulating the large hydrolysis equipment of the actual production line.
2. The experimental method comprises the following steps: firstly, an on-line production hydrolysis device is adopted to operate according to the hydrolysis treatment method and relevant hydrolysis conditions in the embodiment 1 to prepare an on-line production sample 1; then, the chlor-alkali ion exchange membrane obtained in example 1 and the on-line production sample 1 were subjected to an electrolysis test, respectively, and the test results were compared.
3. And (4) experimental conclusion: the results of the experiment are shown in table 1.
Table 1 comparison of the performance of the chlor-alkali ion exchange membrane obtained in example 1 with that of sample 1 produced on-line
As can be seen by comparison of table 1, the average electrolytic voltage of the ion-exchange membrane prepared in example 1 was 2.978V, and the standard deviation was 0.004; the voltage of sample 1 produced on line averaged 2.987V with a standard deviation of 0.002. The stability of the two is equivalent, the average value is only 0.009V different, and the performance of the membrane obtained by the method of the utility model is considered to be equivalent to that of the on-line production membrane. Therefore, through the utility model discloses a small-size perfluoro ion exchange membrane reactor for hydrolytic transformation carries out membrane hydrolytic transformation research experiment, obtained optimization data can be directly applied to the large-scale production facility of hydrolysising on the serialization production line, need not to carry on pilot scale again etc..
Experimental example 2
1. The purpose of the experiment is as follows: test the reactor for hydrolysis and transformation of the small perfluorinated ion exchange membrane of the utility model to simulate the actual production
Precision of large-scale hydrolysis equipment.
2. The experimental method comprises the following steps: firstly, an on-line production hydrolysis device is adopted to operate according to the hydrolysis treatment method and relevant hydrolysis conditions in the embodiment 2 to prepare an on-line production sample 2; then, the chlor-alkali ion exchange membrane obtained in example 2 and the on-line production sample 2 were subjected to an electrolytic test, respectively, and the test results were compared.
3. The experimental conclusion is that: the results of the experiment are shown in table 2.
Table 2 comparison of performance of chlor-alkali ion exchange membranes obtained in example 2 with that of sample 2 produced on line
As can be seen by comparison of table 2, the average electrolytic voltage of the ion-exchange membrane prepared in example 2 was 3.027V, with a standard deviation of 0.005; the voltage for sample 2 produced on-line averaged 3.038V with a standard deviation of 0.003. The stability of the two is equivalent, the average value is only 0.011V, and the performance of the membrane obtained by the method of the utility model is equivalent to that of the on-line production membrane.
Claims (10)
1. A small reactor for hydrolysis transformation of a perfluorinated ion exchange membrane is characterized by comprising a reaction tank, a circulating pump, an ion exchange membrane hanger and a placing rack matched with the inner size of the reaction tank; a heating device, a temperature measuring device and a hydrolysate circulating pipeline are arranged in the reaction tank, wherein the hydrolysate circulating pipeline is connected with a circulating pump; the placing frame is independent of the reaction tank; limiting grooves for fixing the ion exchange membrane hanging rack are symmetrically arranged on two sides in the placing rack; the ion exchange membrane hanger comprises a spring, a needle plate, an outer frame matched with the size of the placing frame and a needle plate fixing plate arranged in the outer frame; a positioning plate is arranged on the outer side of the outer frame and corresponds to the limiting groove of the placing frame; the four edges of the outer frame are provided with spring fixing holes; the number of the needle plate fixing plates is 4, a spring fixing hole is arranged on one long edge of each needle plate fixing plate, and when the needle plate fixing plate is used, the needle plate fixing plates are connected with the outer frame through the springs and the spring fixing holes; a needle plate fixing hole for fixing the needle plate is arranged on the other long edge of each needle plate fixing plate; two short side ends of each needle plate fixing plate are respectively provided with a connecting hole for fixedly connecting 4 needle plate fixing plates; the needle plate comprises a needle and a base, wherein the base of the needle plate is provided with a needle plate fixing hole, and the needle plate fixing hole corresponds to a needle plate fixing hole formed in the needle plate fixing plate.
2. The reactor for hydrolysis transformation of the small perfluorinated ion exchange membrane as claimed in claim 1, wherein the rotation speed of the circulating pump is 2750-3150 rpm, the flow rate is 13-15L/min, the power is 70-90W, and the rated voltage is 220V; the heating device is an electric heating pipe; the temperature measuring device is a thermocouple.
3. The reactor for hydrolysis conversion of a small perfluoro ion exchange membrane according to claim 2 wherein the electric heating tube extends downward to the bottom of the reaction tank along the inner wall of the narrow side of the reaction tank and is uniformly laid on the bottom of the reaction tank; the distance between the electric heating pipe and the inner wall of the narrow side is less than or equal to 50mm; the number of the thermocouples is at least 1, and the thermocouples are arranged at the position which is less than or equal to 1000mm away from the bottom of the reaction tank.
4. The reactor for hydrolysis transformation of the small-sized perfluorinated ion exchange membrane as claimed in claim 1, wherein the liquid inlet of the hydrolysate circulating pipeline is fixed at a position which is not more than 200mm away from the top of the reaction tank; the liquid outlet is fixed at the position which is less than or equal to 200mm away from the bottom of the reaction tank.
5. The reactor for hydrolysis conversion of a small-sized perfluorinated ion exchange membrane according to claim 1, wherein the height of the inner dimension of the reaction tank is as follows: length: the width is 1-10.
6. The reactor for hydrolysis transformation of a small-sized perfluorinated ion exchange membrane according to claim 1, wherein the limiting grooves are symmetrically arranged in a group at two sides; each group of adjacent limiting grooves are equidistant; a limiting plate is arranged in the limiting groove.
7. The reactor for hydrolysis conversion of a small perfluoro ion exchange membrane according to claim 1 wherein a handle is provided above the rack.
8. The reactor for hydrolysis conversion of a miniature perfluorinated ion exchange membrane according to claim 1, wherein the outer frame has a square shape.
9. The reactor for hydrolysis transformation of a small-sized perfluorinated ion exchange membrane as claimed in claim 1, wherein the tension of the spring is in the range of 0.1 to 100N.
10. The reactor for hydrolysis transformation of a small-sized perfluorinated ion exchange membrane according to claim 1, wherein the length of the needle is 2 to 20mm; the needles are distributed on the base in 1-3 rows, and the included angle between the needles and the needle plate fixing plate is more than or equal to 45 degrees and less than 90 degrees.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115337965A (en) * | 2022-07-07 | 2022-11-15 | 山东东岳高分子材料有限公司 | An experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115337965A (en) * | 2022-07-07 | 2022-11-15 | 山东东岳高分子材料有限公司 | An experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device |
| CN115337965B (en) * | 2022-07-07 | 2024-12-17 | 山东东岳高分子材料有限公司 | Experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device |
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