An experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device

Abstract

The present invention belongs to the technical field of ion exchange membranes, and specifically relates to an experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device comprises a circulation pump, a reaction tank, a plate frame and a tension frame. The hydrolysis transformation reaction device can complete the hydrolysis transformation reaction of perfluorinated ion exchange membranes of various specific experimental sizes, is suitable for studying the hydrolysis transformation reaction parameters of perfluorinated ion exchange membranes, and provides scientific and reliable technical indicators for optimizing the hydrolysis transformation process parameters of perfluorinated ion exchange membranes in industrial production.

Description

Technical Field

[0001] The invention belongs to the technical field of ion exchange membranes, and specifically relates to an experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device. Background Art

[0002] Currently, the perfluorinated ion exchange membrane used in the chlor-alkali industry includes two or more layers of fluorinated polymers, reinforced fibers and hydrophilic coatings. The fluorinated polymer layers are connected by a special cross-linking structure. The functional groups include -CO2M and -SO3M, and M can be H, Li, Na, K, etc.

[0003] During the processing of perfluorinated ion exchange membrane, its precursor does not have ion exchange capacity. In order to obtain ion exchange capacity, the precursor needs to undergo a hydrolysis transformation process in an alkaline solution to convert -SO2F and -COOCH3 groups into -SO3 - M + and -COO - M + The hydrolysis reaction of the group is as follows:

[0004] R f -SO2F+2MOH→R f -SO3 - M + +H2O (1)

[0005] R f -COOCH3+2MOH→R f -COO - M + +CH3OH (2)

[0006]

[0007] While undergoing the hydrolysis transformation, the mixed nano sacrificial materials in the membrane are decomposed, wherein the nano sacrificial fibers are decomposed to form nano channels in the membrane, and the nano inorganic particles are decomposed to form nano holes in the membrane.

[0008] It can be seen that the hydrolysis transformation of perfluorinated ion exchange membrane plays a key role in the ion exchange function of the membrane. Therefore, in order to achieve the purpose of optimizing the ion transfer performance of perfluorinated ion exchange membrane, it is particularly important to optimize the process parameters of hydrolysis transformation of perfluorinated ion exchange membrane in industrial production.

[0009] However, in the actual production of perfluoro ion exchange membranes, the hydrolysis transformation process is a continuous production process, which generally requires the support of larger production equipment. Large-scale equipment for continuous production is mobile processing in the form of membrane rolls, generally 300 to 400 meters per roll, and 1400 to 2000 mm in width; this scale of membrane rolls consumes at least tens of kilograms, or even hundreds of kilograms, of alkali solution and other raw material solutions during the hydrolysis transformation process. If actual production equipment is used to optimize the process parameters of the hydrolysis transformation of perfluoro ion exchange membranes, not only is the operation complicated and cumbersome, but more importantly, it is time-consuming and consumable, especially a waste of raw materials. However, there is no special experimental reaction device for the hydrolysis transformation of perfluoro ion exchange membranes in the prior art, which is suitable for research experiments on optimizing membrane hydrolysis transformation. Summary of the invention

[0010] The purpose of the present invention is to provide an experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device, by which perfluorinated ion exchange membrane hydrolysis transformation reactions of various specific experimental sizes can be completed, which is suitable for studying the perfluorinated ion exchange membrane hydrolysis transformation reaction parameters and providing scientific and reliable technical indicators for optimizing the perfluorinated ion exchange membrane hydrolysis transformation process parameters in industrial production.

[0011] In the process of developing an experimental hydrolysis transformation reaction device, the inventor discovered that in the actual continuous production process of perfluoro ion exchange membranes, the perfluoro ion exchange membranes will be affected by various forces during the hydrolysis transformation, mainly tension and solution circulation force. Therefore, if the above-mentioned research experiment on ion exchange membranes is to be more scientific, it is necessary to comprehensively consider the various external force factors that the perfluoro ion exchange membranes are subjected to in the actual production of hydrolysis transformation process. That is, the reaction device used needs to simulate the various external forces that the ion exchange membranes are subjected to in the actual hydrolysis transformation production as much as possible, and complete the experimental research based on this. How to simulate the external forces that the ion exchange membranes are subjected to in the continuous production of hydrolysis transformation in a non-continuous experimental reaction device as close to reality as possible, including the type of force and the magnitude of the force, has become a technical difficulty in the development of the device.

[0012] The inventors have overcome the above technical difficulties through their creative work and obtained the following technical solutions. The specific technical solutions are as follows:

[0013] An experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device comprises a circulation pump, a reaction tank, a plate frame and a tension frame; the rotation speed of the circulation pump is 2750-3150rpm, the flow rate is 13-15L / min, the power is 70-90W, and the rated voltage is 220V; a heating component, a temperature measuring component and a liquid circulation pipeline are installed in the reaction tank, wherein the liquid circulation pipeline is connected to the circulation pump; the plate frame is a detachable frame matching the internal size of the reaction tank, and limit grooves for fixing the tension frame are symmetrically arranged on both sides of the frame; the tension frame comprises a spring, a needle plate, a support frame matching the size of the plate frame, and a needle plate fixing plate arranged in the support frame; a positioning plate is arranged on the outer side of the support frame, and the positioning plate and the plate frame are fixed to each other. The support frame has a limit groove corresponding to the support frame; spring fixing holes are provided on the four sides of the support frame; there are 4 needle plate fixing plates, and a spring fixing hole is provided on one of the long sides of each needle plate fixing plate. When in use, the needle plate fixing plate is connected to the support frame through the spring and the spring fixing hole; a needle plate fixing hole for fixing the needle plate is provided on the other long side of each needle plate fixing plate; connecting holes for fixing and connecting 4 needle plate fixing plates are respectively provided at the two short side ends of each needle plate fixing plate; the needle plate for fixing the perfluorinated ion exchange membrane includes a needle and a base, wherein the angle between the needle and the needle plate fixing plate is greater than or equal to 45° and less than 90°; a needle plate fixing hole is provided on the base of the needle plate, and the needle plate fixing hole corresponds to the needle plate fixing hole provided on the needle plate fixing plate.

[0014] The circulating pump in the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device is made of PVDF, and its inner cavity is coated with PTFE. The circulating pump has the characteristics of acid and alkali resistance and high temperature resistance, so as to adapt to many process parameter research experiments of perfluorinated ion exchange membrane hydrolysis transformation.

[0015] The heating component adopts an electric heating tube; the temperature measuring component adopts a thermocouple.

[0016] The electric heating tube in the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device extends downward along the narrow side inner wall of the reaction tank to the bottom of the reaction tank and is evenly laid on the bottom of the reaction tank, which is conducive to uniform heating of the hydrolysis reaction liquid.

[0017] The distance between the electric heating tube and the inner wall of the narrow side is ≤50mm; the outer diameter of the electric heating tube is 5-20mm, and the inner diameter is 3-18mm. With this design, not only can the solution be heated efficiently, but also the volume occupied in the reaction tank is smaller.

[0018] There is at least one thermocouple installed at a distance of ≤1000mm from the bottom of the reaction tank. This design ensures that the volume occupied in the reaction tank is minimized while also ensuring accurate measurement of the true temperature of the hydrolysis solution in the reaction tank, avoiding the influence of the metal thermal conductivity of the reaction tank on the measurement data. After all, the process parameters of the hydrolysis transformation are being studied and optimized, so the accuracy of data measurement is very important for the scientific reliability of the research.

[0019] Preferably, the thermocouple is installed at a position 50 to 800 mm away from the bottom of the reaction tank; more preferably, the thermocouple is installed at a position 80 to 500 mm away from the bottom of the reaction tank.

[0020] The liquid inlet of the liquid circulation pipeline in the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device is fixed at a position ≤200 mm away from the top of the reaction tank; the liquid outlet is fixed at a position ≤200 mm away from the bottom of the reaction tank; the portion of the liquid circulation pipeline located outside the reaction tank has an outer diameter of 5 to 20 mm and an inner diameter of 3 to 18 mm, and is connected to a circulation pump through a hose with an outer diameter of 3 to 18 mm and an inner diameter of 1 to 16 mm.

[0021] The internal dimensions of the reaction tank in the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device are height: length: width of 1-10:1-10:1-2.5.

[0022] Preferably, the internal dimensions of the reaction tank are 200-1000 mm in height, 200-1000 mm in length, and 100-500 mm in width. The above size range is designed according to the actual needs of the hydrolysis transformation reaction, and fully meets the hydrolysis reaction of perfluorinated ion exchange membranes of various specific sizes, and will not be too large to cause waste of materials, etc., and will not be too small to be applicable to ion exchange membranes of larger sizes. The designed reaction tank is fully suitable for laboratory research on perfluorinated ion exchange membrane hydrolysis reaction parameters.

[0023] The limiting grooves in the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device are arranged in a group symmetrically on both sides, with a total of 1 to 10 groups, which can be used to fix 1 to 10 tension frames; the adjacent limiting grooves in each group are equidistant; the groove depth of the limiting groove is 1 to 15 mm, and the groove width is 1 to 15 mm; a limiting plate is provided in the limiting groove to further fix the position of the tension frame; the width of the positioning plate is 1 to 15 mm, and the thickness is 1 to 15 mm.

[0024] The plate frame in the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device has a length of 150-850 mm, a width of 50-450 mm, and a height of 150-950 mm; the material is selected from one of 304, 310, 310s, 316 or 316L stainless steel grades.

[0025] Preferably, a handle is provided above the plate rack to facilitate the placement and removal of the plate rack in the reaction tank, wherein the height of the handle is 50-200 mm and the width is 50-200 mm. The material of the handle can be selected from 304, 310, 310s, 316, 316L stainless steel or copper or iron electroplated stainless steel.

[0026] The support frame in the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device is square, the outer width of the support frame is 150-850 mm, the outer length is 150-950 mm, the thickness is 1-50 mm, the inner width of the support frame is 100-840 mm, the inner length is 120-920 mm. The material of the support frame can be selected from one of 304, 310, 310s, 316, 316L stainless steel or copper or iron electroplated stainless steel.

[0027] The thickness of the four pin plate fixing plates in the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device is 1 to 50 mm; the length of two pin plate fixing plates is 115 to 915 mm, and the two pin plate fixing plates in this length range serve as the upper and lower horizontal edges; the length of the other two pin plate fixing plates is 95 to 835 mm, and the two pin plate fixing plates in this length range serve as the left and right vertical edges. The material of the pin plate fixing plate can be selected from one of 304, 310, 310s, 316, 316L stainless steel grades or copper or iron electroplated stainless steel.

[0028] The number of the spring fixing holes arranged on each side of the support frame and the number of the spring fixing holes arranged on the needle plate fixing plate are both 1 to 20; and the diameter of the spring fixing holes are both 1 to 10 mm.

[0029] The structural design of the above-mentioned support frame and needle plate fixing plate, including the dimensions, is based on the characteristics of the perfluorinated ion exchange membrane that is being tested for performance.

[0030] The number of the needle plate fixing holes is 2 to 10, which are used to fix the needle plate; the tension range of the spring is 0.1 to 100 N. The material of the spring can be selected from one of 304, 310, 310s, 316, and 316L stainless steel grades.

[0031] The length of the base in the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device is 20-880 mm, the width is 5-30 mm; the length of the needle is 2-20 mm; the number of needles contained in each needle plate is 1-440; the needles are distributed on the base in 1-3 rows. The material of the needle plate can be selected from one of 304, 310, 310s, 316, 316L stainless steel or copper or iron electroplated stainless steel.

[0032] The beneficial effects of the present invention are as follows: the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device designed by the present invention is a discontinuous type, that is, it can process perfluorinated ion exchange membrane experimental samples one by one, which is more suitable for experimental research. The minimum specification of the ion exchange membrane that can be processed by the reaction device can be up to 5×20mm, and the application range is wide. It includes a circulation pump, a reaction tank, a plate rack and a tension rack; the speed of the circulation pump is 2750-3150rpm, the flow rate is 13-15L / min, the power is 70-90W, and the rated voltage is 220V;

[0033] First, in order to accurately simulate the solution circulation force exerted on the perfluoro ion exchange membrane during the hydrolysis transformation in actual production, the inventors discovered through innovative research that by designing the circulation pump and the relevant parameters of the circulation pump to the range values ​​in the above technical scheme, it is possible to completely simulate the circulation force of the hydrolysis solution exerted on the membrane during the actual production process, thereby introducing this force factor into the research experiment on the optimization of the hydrolysis transformation process parameters, thereby making the research results more in line with actual production, more scientific and effective.

[0034] At the same time, in order to simulate the tension effect of large-scale hydrolysis transformation equipment on the membrane in actual production, the inventor creatively designed a tension frame composed of a spring, a needle plate, a support frame and a needle plate fixing plate. The linkage relationship between these components simulates the tension caused by large equipment on the membrane. In particular, the design of the spring is more flexible and can simulate the tension caused by different models of large equipment in actual production.

[0035] The inventors also took into account that during the hydrolysis transformation reaction of the perfluoro ion exchange membrane, the ion membrane will swell and increase in size, so the angle between the needle in the needle plate used to fix the perfluoro ion exchange membrane and the needle plate fixing plate is designed to be greater than or equal to 45° and less than 90°; if it is not within this range, for example, the needle and the needle plate fixing plate are at a right angle or an obtuse angle, the ion exchange membrane is very likely to fall off during the reaction; but if the angle between the needle and the needle plate fixing plate is too small, when fixing the ion exchange membrane, it is difficult for the membrane body to pass through the needle, the operation difficulty increases, and it is easy to cause artificial damage to the membrane, bringing some unknown influencing factors, which may lead to inaccuracy in the research parameters.

[0036] Combined with the above design, the basic principle of using the device described in the present invention to conduct research experiments is as follows: fix the perfluoro ion exchange membrane on the needle plate fixing plate with the needle on the needle plate, and then use the spring to connect the needle plate fixing plate and the support frame. At this time, remove the screws previously used to connect and fix the needle plate fixing plate in the horizontal and vertical directions, so that the needle plate fixing plate drives the needle plate, and then drives the perfluoro ion exchange membrane to be subjected to the tension simulated by the spring, thereby simulating the tension of the equipment on the membrane during the actual production process. The size of the tension can be adjusted by adjusting the model of the spring; fix the tension frame with the membrane on the plate frame, put it into the reaction tank filled with constant temperature solution as a whole, and turn on the circulation pump to simulate the solution circulation system in the equipment tank during the actual production process. The above can complete the simulation of the hydrolysis process in actual production, and use this as a basis to complete the research work in the laboratory.

[0037] Compared with conducting research experiments on large-scale production equipment, the advantages of the present invention are:

[0038] (1) Saving raw material costs. Since the hydrolysis reaction device of the present invention has a small volume, the amount of solution raw materials and perfluorinated ion exchange membrane raw materials required for experimental research is less;

[0039] (2) The operation method is simple and easy, and there is no need to modify the existing equipment and production line, which will not affect normal production. Although the reaction device of the present invention has no similarity in appearance with the actual production equipment, the perfluorinated ion exchange membrane samples tested can be subjected to effects similar to those of the production line equipment, such as tension and solution circulation force, so that the final research results are more practical. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1 It is a schematic diagram of the three-dimensional structure of an experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device in a specific embodiment of the present invention.

[0041] Figure 2 It is a top view of an experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device in a specific embodiment of the present invention.

[0042] Figure 3 It is a schematic diagram of the three-dimensional structure of the reaction tank in the reaction device in a specific embodiment of the present invention.

[0043] Figure 4 It is a front view of the reaction tank in the reaction device in a specific embodiment of the present invention.

[0044] Figure 5 It is a left view of the reaction tank in the reaction device in the specific implementation manner of the present invention.

[0045] Figure 6 It is a top view of the reaction tank in the reaction device in a specific embodiment of the present invention.

[0046] Figure 7 It is a schematic diagram of the three-dimensional structure of the plate frame in the reaction device in a specific implementation manner of the present invention.

[0047] Figure 8 for Figure 7 A partial enlarged view of the middle limit groove.

[0048] Fig. 9 It is a front view of the plate rack in the reaction device in a specific embodiment of the present invention.

[0049] Fig.10 It is a left view of the plate rack in the reaction device in the specific implementation manner of the present invention.

[0050] Fig.11 It is a top view of the plate rack in the reaction device in a specific embodiment of the present invention.

[0051] Fig.12 It is a schematic diagram of the three-dimensional structure of the tension frame in the reaction device in a specific implementation manner of the present invention.

[0052] Fig.13 It is a front view of the tension frame in the reaction device in a specific implementation manner of the present invention.

[0053] Fig.14 It is a left view of the tension frame in the reaction device in the specific implementation manner of the present invention.

[0054] Fig.15 It is a top view of the tension frame in the reaction device in a specific embodiment of the present invention.

[0055] Fig.16 It is a front view of the support frame in the reaction device in a specific embodiment of the present invention.

[0056] Fig.17 It is a left view of the support frame in the reaction device in a specific embodiment of the present invention.

[0057] Fig.18 It is a schematic diagram of the three-dimensional structure of the needle plate fixing plate located in the vertical direction in the reaction device in the specific implementation manner of the present invention.

[0058] Fig.19 It is a front view of a needle plate fixing plate located in a vertical direction in the reaction device in a specific embodiment of the present invention.

[0059] Fig. 20 It is a schematic diagram of the three-dimensional structure of the needle plate fixing plate located in the horizontal direction in the reaction device in the specific implementation manner of the present invention.

[0060] Fig.21It is a front view of a needle plate fixing plate located in a horizontal direction in the reaction device in a specific embodiment of the present invention.

[0061] Fig. 22 It is a top view of a needle plate fixing plate located in a horizontal direction in the reaction device in a specific embodiment of the present invention.

[0062] Among them, 1 is an electric heating tube, 2 is a thermocouple, 3 is a liquid circulation pipeline, 4 is a limit groove, 5 is a limit plate, 6 is a handle, 7 is a support 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 plate frame. DETAILED DESCRIPTION

[0063] The technical solution of the present invention is described in detail below in conjunction with the accompanying drawings. Many materials and operating methods used in the experiment of the present invention are well known in the art, but the present invention is still described as detailed as possible here.

[0064] The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device comprises a circulation pump, a reaction tank, a plate frame 14 and a tension frame.

[0065] The circulation pump has a rotation speed of 2750-3150 rpm, a flow rate of 13-15 L / min, a power of 70-90 W, and a rated voltage of 220 V. The circulation pump in the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device is made of PVDF, and its inner cavity is coated with PTFE.

[0066] The internal dimensions of the reaction tank are height: length: width of 1-10:1-10:1-2.5; preferably, the internal dimensions of the reaction tank are height 200-1000mm, length 200-1000mm, and width 100-500mm.

[0067] An electric heating tube 1, a thermocouple 2 and a liquid circulation pipeline 3 are installed in the reaction tank.

[0068] The electric heating tube 1 extends downward along the narrow side inner wall of the reaction tank to the bottom of the reaction tank and is evenly laid on the bottom of the reaction tank. The distance between the electric heating tube 1 and the narrow side inner wall is ≤50mm; the outer diameter of the electric heating tube 1 is 5-20mm, and the inner diameter is 3-18mm. The laying route of the electric heating tube 1 forms the following view in the reaction tank: Figure 4 As shown, in the front view, the electric heating tube 1 is similar to an "L" shape in the reaction tank; Figure 5 As shown, in the left view, the electric heating tube 1 is similar to a "U" shape in the reaction tank; Figure 6 As shown, the electric heating tube 1 is similar to a "U" shape in the reaction tank in the top view. The outer wall spacing of the "U" shaped heating tube is ≤490mm.

[0069] There is at least one thermocouple 2, one of which can be installed at the bottom of the reaction tank and one below the liquid level of the hydrolysis solution. The thermocouple 2 can be installed in a direction parallel to, perpendicular to, or at a certain angle to the bottom of the reaction tank.

[0070] The thermocouple 2 is installed at a distance of ≤1000 mm from the bottom of the reaction tank; preferably, the thermocouple 2 is installed at a distance of 50 to 800 mm from the bottom of the reaction tank; more preferably, the thermocouple 2 is installed at a distance of 80 to 500 mm from the bottom of the reaction tank.

[0071] The liquid inlet of the liquid circulation pipeline 3 is fixed at a position ≤200mm away from the top of the reaction tank; the liquid outlet is fixed at a position ≤200mm away from the bottom of the reaction tank; the part of the liquid circulation pipeline 3 located outside the reaction tank has an outer diameter of 5-20mm and an inner diameter of 3-18mm, and is connected to the circulation pump through a hose with an outer diameter of 3-18mm and an inner diameter of 1-16mm.

[0072] The plate frame 14 is a frame that matches the internal dimensions of the reaction tank and is independent of the reaction tank, and can be flexibly placed, taken out and disassembled. The frame has symmetrically arranged limit grooves 4 for fixing the tension frame on both sides. The limit grooves 4 are arranged in a group with symmetry on both sides, and there are 1 to 10 groups in total, which can be used to fix 1 to 10 tension frames; each group of adjacent limit grooves 4 is equidistant; the limit grooves 4 have a groove depth of 1 to 15 mm and a groove width of 1 to 15 mm; a limit plate 5 is arranged in the limit groove 4 to further fix the position of the tension frame.

[0073] The plate frame 14 has a length of 150-850 mm, a width of 50-450 mm, and a height of 150-950 mm; the material is selected from one of 304, 310, 310s, 316 or 316L stainless steel grades;

[0074] A handle 6 is provided above the plate rack 14 to facilitate the placement and removal of the plate rack in the reaction tank, wherein the handle 6 has a height of 50-200 mm and a width of 50-200 mm. The material of the handle 6 can be selected from one of 304, 310, 310s, 316, 316L stainless steel or copper or iron electroplated stainless steel.

[0075] The tension frame comprises a spring, a needle plate 9 , a support frame 7 having a size matching that of the plate frame 14 , and a needle plate fixing plate 8 placed in the support frame 7 .

[0076] The support frame 7 is square, the outer width of the support frame 7 is 150-850 mm, the outer length is 150-950 mm, the thickness is 1-50 mm, the inner width of the support frame 7 is 100-840 mm, and the inner length is 120-920 mm. The material of the support frame 7 can be selected from one of 304, 310, 310s, 316, 316L stainless steel or copper or iron electroplated stainless steel.

[0077] A positioning plate 10 is provided on the outer side of the support frame 7. The positioning plate 10 corresponds to the plate frame limiting groove 4. The positioning plate 10 has a width of 1 to 15 mm and a thickness of 1 to 15 mm. The four sides of the support frame 7 are each provided with 1 to 20 spring fixing holes 11.

[0078] There are four needle plate fixing plates 8, all with a thickness of 1 to 50 mm; two of the needle plate fixing plates 8 have a length of 115 to 915 mm, and the two needle plate fixing plates 8 in this length range serve as upper and lower horizontal edges; the total length of the needle plate fixing plates 8 in the horizontal direction with spring fixing holes is 1 to 875 mm.

[0079] The lengths of the other two needle plate fixing plates 8 are both 95-835 mm, and the two needle plate fixing plates 8 in this length range serve as the left and right vertical edges. The total length of the spring fixing holes on the needle plate fixing plates 8 in the vertical direction is 1-795 mm.

[0080] The material of the needle plate fixing plate 8 can be selected from one of 304, 310, 310s, 316, 316L stainless steel grades or copper or iron electroplated stainless steel.

[0081] One long edge of each needle plate fixing plate 8 is provided with 1 to 20 spring fixing holes 11. When in use, the needle plate fixing plate 8 is connected to the support frame 7 through the springs and the spring fixing holes 11; the other long edge of each needle plate fixing plate 8 is provided with a needle plate fixing hole 12 for fixing the needle plate 9.

[0082] Each of the two short side ends of each needle plate fixing plate 8 is provided with a connection hole 13 for fixing and connecting the four needle plate fixing plates 8. The needle plate fixing plates 8 in the horizontal direction and the vertical direction are fixed to each other through the connection holes 13. When the four needle plate fixing plates are surrounded in a "U" shape, the spring fixing hole 11 is outside the "U" shape, and the needle plate fixing hole 12 is inside the "U" shape.

[0083] like Figure 20-22 As shown, the needle plate fixing plate 8 located in the horizontal direction is overall "convex" shaped, and the needle plate fixing plate 8 with the spring fixing hole 11 in the middle is higher than the needle plate fixing plate 8 with the connecting holes 13 on both sides by the thickness of the needle plate fixing plate.

[0084] The diameter of the spring fixing holes 11 is 1-10 mm.

[0085] The needle plate 9 for fixing the perfluorinated ion exchange membrane comprises needles and a base. The base has a length of 20 to 880 mm and a width of 5 to 30 mm; the needles have a length of 2 to 20 mm; each needle plate contains 1 to 440 needles; the needles are arranged in 1 to 3 rows in the length direction of the base. The material of the needle plate can be selected from one of 304, 310, 310s, 316, 316L stainless steel or copper or iron electroplated stainless steel.

[0086] The angle between the needle and the needle plate fixing plate 8 is greater than or equal to 45° and less than 90°.

[0087] 2 to 10 needle plate fixing holes 12 for fixing the needle plate are provided on the base of the needle plate 9, and the needle plate fixing holes correspond to the needle plate fixing holes provided on the needle plate fixing plate.

[0088] The tension range of the spring is 0.1 to 100 N. The material of the spring can be selected from one of 304, 310, 310s, 316, and 316L stainless steel grades.

[0089] Example 1

[0090] The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device A has a reaction tank made of 310s stainless steel, a length of 480 mm, a width of 250 mm, and a height of 450 mm. The internal electric heating tube 1 is distributed in a "U" shape on the inner wall of one side of the width direction of the reaction tank and the bottom of the reaction tank, and the side surface is "L" shaped as a whole. Two thermocouples 2 are respectively installed on the side walls in the width direction at a distance of 100 mm and 390 mm from the bottom of the reaction tank, and the direction is 90° with the side walls in the width direction of the reaction tank. 25% NaOH+10% DMSO 28.5 kg is prepared in the laboratory and added to the reaction tank. The temperature is adjusted to 70°C, and the PVDF material circulation pump coated with PTFE in the inner cavity is turned on to circulate the solution. The rotation speed is 2750 rpm, the flow rate is 15 L / min, the power is 90 W, the rated voltage is 220 V, and the temperature is kept constant for half an hour.

[0091] A copper-plated stainless steel needle plate 9 with a length of 190 mm and a width of 20 mm is fixed to a needle plate fixing plate 8 placed in a horizontal direction by screws, wherein the side length of the needle plate fixing plate 8 in the horizontal direction is 250 mm; a copper-plated stainless steel needle plate 9 with a length of 160 mm and a width of 20 mm is fixed to a needle plate fixing plate 8 placed in a vertical direction by screws, wherein the side length of the needle plate fixing plate 8 in the vertical direction is 220 mm.

[0092] Then, the needle plate fixing plates placed in the horizontal direction and the needle plate fixing plates placed in the vertical direction are fixed in pairs by screws to form a rectangle.

[0093] The hydrolysis precursor chlor-alkali ion exchange membrane sampled from continuous production was cut into 200 mm long and 180 mm wide samples, a total of 5 pieces, fixed to the needle plate, and the four sides of the needle plate fixing plate 8 were connected to the four sides of the supporting frame 7 using 10N 316 stainless steel springs, with two springs on each side; the screws fixing the needle plate fixing plate in the horizontal and vertical directions were removed so that the membrane was fully subjected to the tension from the springs.

[0094] Insert the above five groups of support frames 7 with fixed membranes into the plate frame 14 along the limiting groove 4. The plate frame 14 has a length of 400 mm, a width of 220 mm, a height (without the handle part) of 300 mm, and a height of the handle 6 of 100 mm. A total of 5 groups of support frames can be inserted.

[0095] The plate rack 14 is placed in a hydrolysis reaction tank as a whole and covered with a 310s stainless steel cover. After reacting for 60 minutes, the plate rack 14 is removed, the hydrolyzed membrane is taken down, and the surface is washed with water to obtain 5 chlor-alkali ion exchange membranes with ion exchange capacity.

[0096] Example 2

[0097] The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device B is prepared in the laboratory with 20% NaOH + 5% DMSO 18.3 kg, added to the reaction tank, and the temperature is adjusted to 70° C. The rest is the same as the reaction device A in Example 1, except that the reaction tank of the reaction device B is 480 mm long, 160 mm wide, and 450 mm high.

[0098] The hydrolysis precursor chlor-alkali ion exchange membrane sampled from the continuous production was cut into 200 mm long and 180 mm wide samples, a total of 3 pieces, and fixed to the needle plate.

[0099] Insert the above three groups of support frames with fixed membranes into the plate rack along the limiting grooves. The plate rack 14 has a length of 400 mm, a width of 150 mm, a height (without the handle part) of 300 mm, and a height of 100 mm for the handle 6. A total of 3 groups of support frames can be inserted.

[0100] The plate rack 14 is placed in a hydrolysis reaction tank as a whole, covered with a 310s stainless steel cover, and after reacting for 60 minutes, the plate rack is removed, the hydrolyzed membrane is taken down, and the surface is washed with water to obtain three chlor-alkali ion exchange membranes with ion exchange capacity.

[0101] Experimental Example 1

[0102] 1. Experimental purpose: To test the accuracy of the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device of the present invention in simulating the large-scale hydrolysis equipment of the actual production line.

[0103] 2. Experimental method: First, an online production hydrolysis equipment is used to operate according to the hydrolysis treatment method and related hydrolysis conditions in Example 1 to obtain an online production sample 1; then the chlor-alkali ion exchange membrane obtained in Example 1 and the online production sample 1 are subjected to electrolysis tests respectively, and the test results are compared.

[0104] 3. Experimental conclusion: The experimental results are shown in Table 1.

[0105] Table 1 Performance comparison of the chlor-alkali ion exchange membrane obtained in Example 1 and the online production sample 1

[0106]

[0107] From the comparison in Table 1, it can be seen that the average electrolysis voltage of the ion exchange membrane prepared in Example 1 is 2.978V, and the standard deviation is 0.004; the voltage of the online production sample 1 is 2.987V on average, and the standard deviation is 0.002. The stability of the two is comparable, and the average values ​​differ by only 0.009V. It is believed that the membrane performance obtained by the method of the present invention is comparable to that of the online production membrane. It can be seen that the membrane hydrolysis transformation research experiment is carried out by the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device described in the present invention, and the obtained optimization data can be directly applied to the large-scale hydrolysis production equipment on the continuous production line without the need for pilot testing.

[0108] Experimental Example 2

[0109] 1. Experimental purpose: To test the accuracy of the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device of the present invention in simulating the large-scale hydrolysis equipment of the actual production line.

[0110] 2. Experimental method: First, the online production hydrolysis equipment is used to operate according to the hydrolysis treatment method and related hydrolysis conditions in Example 2 to obtain the online production sample 2; then the chlor-alkali ion exchange membrane obtained in Example 2 and the online production sample 2 are subjected to electrolysis tests respectively, and the test results are compared.

[0111] 3. Experimental conclusion: The experimental results are shown in Table 2.

[0112] Table 2 Performance comparison of the chlor-alkali ion exchange membrane obtained in Example 2 and the online production sample 2

[0113]

[0114] From the comparison in Table 2, it can be seen that the average electrolysis voltage of the ion exchange membrane prepared in Example 2 is 3.027V, with a standard deviation of 0.005; the voltage of the online production sample 2 is 3.038V on average, with a standard deviation of 0.003. The stability of the two is comparable, with an average value difference of only 0.011V. It is believed that the performance of the membrane obtained by the method of the present invention is comparable to that of the online production membrane.

Claims

1. An experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device, characterized in that: It includes a circulation pump, a reaction tank, a plate rack and a tension rack; the rotation speed of the circulation pump is 2750-3150rpm, the flow rate is 13-15L / min, the power is 70-90W, and the rated voltage is 220V; a heating component, a temperature measuring component and a liquid circulation pipeline are installed in the reaction tank, wherein the liquid circulation pipeline is connected to the circulation pump; the plate rack is a detachable frame matching the internal size of the reaction tank, and limit grooves for fixing the tension rack are symmetrically arranged on both sides of the frame; the tension rack includes a spring, a needle plate, a support frame matching the size of the plate rack, and a needle plate fixing plate placed in the support frame; a positioning plate is arranged on the outside of the support frame, and the positioning plate is aligned with the limit groove of the plate rack Correspondingly; spring fixing holes are provided on the four sides of the support frame; there are 4 needle plate fixing plates, and a spring fixing hole is provided on one of the long sides of each needle plate fixing plate. When in use, the needle plate fixing plate is connected to the support frame through the spring and the spring fixing hole; a needle plate fixing hole for fixing the needle plate is provided on the other long side of each needle plate fixing plate; connecting holes for fixing and connecting the four needle plate fixing plates are provided at the two short side ends of each needle plate fixing plate; the needle plate includes a needle and a base, wherein the angle between the needle and the needle plate fixing plate is greater than or equal to 45° and less than 90°; a needle plate fixing hole is provided on the base of the needle plate, and the needle plate fixing hole corresponds to the needle plate fixing hole provided on the needle plate fixing plate.

2. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 1, characterized in that: The circulating pump is made of PVDF, and its inner cavity is coated with PTFE; the heating component adopts an electric heating tube; and the temperature measuring component adopts a thermocouple.

3. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 2, characterized in that: The electric heating tube extends downward along the narrow side inner wall of the reaction tank to the bottom of the reaction tank and is evenly laid on the bottom of the reaction tank; the distance between the electric heating tube and the narrow side inner wall is ≤50mm; the outer diameter of the electric heating tube is 5-20mm, and the inner diameter is 3-18mm; there is at least one thermocouple, which is installed at a position ≤1000mm away from the bottom of the reaction tank.

4. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 3, characterized in that: The thermocouple is installed at a position 50 to 800 mm away from the bottom of the reaction tank.

5. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 4, characterized in that: The thermocouple is installed at a position 80 to 500 mm away from the bottom of the reaction tank.

6. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 1, characterized in that: The liquid inlet of the liquid circulation pipeline is fixed at a position ≤200mm away from the top of the reaction tank; the liquid outlet is fixed at a position ≤200mm away from the bottom of the reaction tank; the part of the liquid circulation pipeline located outside the reaction tank has an outer diameter of 5-20mm and an inner diameter of 3-18mm, and is connected to the circulation pump through a hose with an outer diameter of 3-18mm and an inner diameter of 1-16mm.

7. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 1, characterized in that: The internal dimensions of the reaction tank are height: length: width of 1-10:1-10:1-2.

5.

8. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 7, characterized in that: The internal dimensions of the reaction tank are 200-1000 mm in height, 200-1000 mm in length, and 100-500 mm in width.

9. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 1, characterized in that: The limit grooves are arranged in a group symmetrically on both sides, with a total of 1 to 10 groups; adjacent limit grooves in each group are equidistant; the limit grooves have a depth of 1 to 15 mm and a width of 1 to 15 mm; a limit plate is provided in the limit groove; the positioning plate has a width of 1 to 15 mm and a thickness of 1 to 15 mm.

10. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 1, characterized in that: The plate rack has a length of 150-850 mm, a width of 50-450 mm, and a height of 150-950 mm; the material is selected from one of 304, 310, 310s, 316 or 316L stainless steel grades.

11. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 10, characterized in that: A handle is arranged above the plate frame, wherein the height of the handle is 50-200 mm and the width is 50-200 mm.

12. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 1, characterized in that: The support frame is square, with an outer width of 150-850 mm, an outer length of 150-950 mm, a thickness of 1-50 mm, an inner width of 100-840 mm, and an inner length of 120-920 mm.

13. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 1, characterized in that: The thickness of the four needle plate fixing plates is 1 to 50 mm; the length of two needle plate fixing plates is 115 to 915 mm, and the length of the other two needle plate fixing plates is 95 to 835 mm; The number of the spring fixing holes provided on each side of the support frame and the number of the spring fixing holes provided on the needle plate fixing plate are both 1 to 20; the diameter of the spring fixing holes are both 1 to 10 mm; The number of the needle plate fixing holes is 2 to 10; the tension range of the spring is 0.1 to 100N.

14. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 1, characterized in that: The base has a length of 20 to 880 mm and a width of 5 to 30 mm; the needles have a length of 2 to 20 mm; each needle plate contains 1 to 440 needles; and the needles are distributed on the base in 1 to 3 rows.

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