CN115337965A - An experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device - Google Patents

Abstract

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

Description

An experimental perfluorinated ion exchange membrane hydrolysis conversion reaction device

technical field

The invention belongs to the technical field of ion exchange membranes, and in particular relates to an experimental type perfluorinated ion exchange membrane hydrolysis transformation reaction device.

Background technique

At present, the perfluorinated ion exchange membrane used in the chlor-alkali industry includes two or more layers of fluoropolymers, reinforcing fibers and hydrophilic coatings. The fluoropolymer layers are connected by a special cross-linking structure, and the functional groups are - CO ₂ M and -SO ₃ M etc., M can be H, Li, Na and K etc.

During the processing of perfluorinated ion exchange membrane, its precursor does not have ion exchange capacity. In order to obtain ion-exchange capability, the precursor needs to undergo a hydrolysis transformation process in alkaline solution to convert -SO ₂ F and -COOCH ₃ groups into -SO ₃ ^- M ⁺ and -COO ^- M ⁺ groups with ion-exchange capability, respectively Group, its hydrolysis reaction formula is as follows:

R _f -SO ₂ F+2MOH→R _f -SO ₃ ^- M ⁺ +H ₂ O (1)

R _f -COOCH ₃ +2MOH→R _f -COO ^- M ⁺ +CH ₃ OH (2)

The mixed nano-sacrifice material in the membrane is decomposed at the same time as the hydrolysis transformation, wherein the nano-sacrifice fiber is decomposed to form nano-holes in the membrane, and the nano-inorganic particles are decomposed to form nano-holes in the membrane.

It can be seen that the hydrolysis transformation of the 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 transport performance of perfluorinated ion exchange membranes, it is particularly important to optimize research experiments on the process parameters of perfluorinated ion exchange membrane hydrolysis transformation in industrial production.

However, in the actual production of perfluorinated ion exchange membranes, the hydrolysis conversion process is a continuous production process, which generally requires relatively large-scale production equipment as a basis. Continuous production of large-scale equipment is carried out in the form of film rolls. Generally, a roll is 300-400 meters long and 1400-2000 mm wide; the scale of film rolls consumes at least dozens of lye and other raw material solutions during the hydrolysis transformation process. kilograms, or even hundreds of kilograms. If the actual production equipment is used to optimize the process parameters of perfluorinated ion exchange membrane hydrolysis transformation, not only the operation is complicated and cumbersome, but more importantly, time-consuming and consumable materials, especially the waste of raw materials. However, in the prior art, there is no special experimental reaction device for hydrolysis transformation of perfluorinated ion exchange membranes, which is suitable for research experiments on optimizing membrane hydrolysis transformation.

Contents of the invention

The purpose of the present invention is to provide an experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device, through which the hydrolysis transformation reaction device can complete the hydrolysis transformation reaction of various specific experimental sizes of perfluorinated ion exchange membranes, suitable for perfluorinated ion exchange The research on the reaction parameters of membrane hydrolysis transformation provides scientific and reliable technical indicators for optimizing the process parameters of perfluorinated ion exchange membrane hydrolysis transformation in industrial production.

In the process of developing the experimental hydrolysis transformation reaction device, the inventors found that in the actual continuous production process of perfluorinated ion exchange membranes, the perfluorinated ion exchange membranes will be affected by various forces when undergoing hydrolysis transformation, mainly tension and solution circulation force, so if you want to make the above research experiments on ion exchange membranes more scientific, you need to take into account all kinds of external force factors that perfluorinated ion exchange membranes are subjected to in the actual production of hydrolysis transformation process, That is to say, the reaction device used needs to simulate the various external forces encountered in the actual hydrolysis transformation production of the ion exchange membrane as much as possible, and complete the experimental research based on this. How to simulate the external force on the ion exchange membrane during the continuous production hydrolysis transformation process in a discontinuous experimental reaction device as close as possible, including the type and magnitude of the force, has become a technology developed by the device. problem.

Through the inventor's creative work, the above-mentioned technical problems have been overcome and the following technical solutions have been obtained. The specific technical solutions are as follows:

An experimental perfluorinated ion exchange membrane hydrolysis conversion reaction device, including a circulating pump, a reaction tank, a plate frame and a tension frame; the rotating speed of the circulating pump is 2750-3150rpm, the flow rate is 13-15L/min, and the power is 70- 90W, rated voltage 220V; heating components, temperature measuring components and liquid circulation pipelines are installed in the reaction tank, wherein the liquid circulation pipeline is connected to the circulation pump; the plate frame is matched with the internal size of the reaction tank The detachable frame is symmetrically provided with limiting slots for fixing the tension frame on both sides of the frame; the tension frame includes a spring, a needle plate, a support frame that matches the size of the plate frame, and a needle placed in the support frame plate fixing plate; the outer side of the support frame is provided with a positioning plate, which corresponds to the limit groove of the plate frame; the four sides of the support frame are provided with spring fixing holes; there are 4 needle plate fixing plates, and each needle plate One of the long edges of the fixing plate is provided with a spring fixing hole. When in use, the needle plate fixing plate is connected with the support frame through the spring and the spring fixing hole; The needle plate fixing hole for fixing the needle plate; the two short side ends of each needle plate fixing plate are respectively provided with connection holes for fixedly connecting 4 needle plate fixing plates; the needles for fixing the perfluorinated ion exchange membrane The 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 arranged on the base of the needle plate, and the needle plate fixing hole and the needle plate fixing plate The set needle plate fixing holes correspond to each other.

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. The circulation pump has the characteristics of acid and alkali resistance and high temperature resistance, so as to adapt to many perfluorinated ion exchange membranes. Research experiment on process parameters of hydrolysis transformation.

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

In the experimental type perfluorinated ion exchange membrane hydrolysis conversion reaction device, the electric heating tube extends down to the bottom of the reaction tank along the narrow inner wall of the reaction tank and is evenly laid on the bottom of the reaction tank, which is beneficial to the uniform heating of the hydrolysis reaction solution.

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

There is at least one thermocouple, which is installed at a position ≤ 1000mm away from the bottom of the reaction tank. This design ensures accurate measurement of the real temperature of the hydrolysis solution in the reaction tank while minimizing the volume occupied in the reaction tank, and avoids the measurement data being affected by the metal heat conduction of the reaction tank. After all, what is studied and optimized is the process parameters of hydrolysis transformation, so the accuracy of data measurement is very important to the scientific reliability of the research.

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

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

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

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, fully satisfying the hydrolysis reaction of perfluorinated ion exchange membranes of various specific sizes, and will not cause waste of materials if it is too large, and it is too small to be suitable for larger size ion exchange membranes. Membrane, the designed reaction tank is fully suitable for laboratory research on the parameters of the hydrolysis reaction of perfluorinated ion exchange membranes.

The limit grooves in the experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device are called a group with two sides symmetrical, 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 equidistant between them; the groove depth of the limiting groove is 1-15mm, and the groove width is 1-15mm; a limiting plate is arranged in the limiting groove for further fixing the position of the tension frame; the width of the positioning plate is 1 ～15mm, the thickness is 1～15mm.

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

Preferably, a handle is provided on the top of the plate frame to facilitate the loading and unloading of the plate frame 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 one of 304, 310, 310s, 316, 316L grade stainless steel or stainless steel plated with copper and iron.

In the experimental type perfluorinated ion exchange membrane hydrolysis transformation reaction device, the supporting frame is square, the outer width of the supporting frame is 150-850 mm, the outer length is 150-950 mm, the thickness is 1-50 mm, and the inner width of the supporting frame is 100-850 mm. 840mm, the inner length is 120~920mm. The material of the supporting frame can be selected from one of 304, 310, 310s, 316, 316L grade stainless steel or copper or iron-plated stainless steel.

The thickness of the four pin plate fixing plates in the experimental perfluorinated ion exchange membrane hydrolysis conversion reaction device is 1-50 mm; the length of the two pin plate fixing plates is 115-915 mm, and the two pin plate fixing plates in this length range The needle plate fixing plate is used as the upper and lower horizontal sides; the length of the other two needle plate fixing plates is 95-835mm, and the two needle plate fixing plates in this length range are used as the left and right vertical sides. The material of the needle plate fixing plate can be selected from one of 304, 310, 310s, 316, 316L grade stainless steel or copper or iron-plated stainless steel.

The number of spring fixing holes on each side of the support frame and the spring fixing holes on the needle plate fixing plate is 1-20; the diameter of the spring fixing holes is 1-10 mm.

The structural design of the above-mentioned supporting frame and the needle plate fixing plate, including the dimensions, are all based on the characteristics of the perfluorinated ion exchange membrane that has been tested for performance.

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

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

The beneficial effects of the present invention are: the experimental type perfluorinated ion exchange membrane hydrolysis conversion reaction device designed in the present invention is a discontinuous type, that is, it can process perfluorinated ion exchange membrane experimental samples one by one, and is better suitable for experimental research. The minimum specification of the ion exchange membrane that the reaction device can handle can be up to 5×20mm, and the scope of application is wide. It includes a circulating pump, a reaction tank, a plate frame and a tension frame; the rotating speed of the circulating pump is 2750-3150rpm, the flow rate is 13-15L/min, the power is 70-90W, and the rated voltage is 220V;

First of all, in order to accurately simulate the solution circulation force experienced by the perfluorinated ion exchange membrane during hydrolysis transformation in actual production, the inventors found through innovative research that the circulation pump and the relevant parameters of the circulation pump were designed to be within the range of the above technical scheme. It can completely simulate the circulation force of the hydrolysis solution on the membrane in the actual production process, so as to introduce this force factor into the research experiment of the optimization of the hydrolysis transformation process parameters, so that the research results are more suitable for the actual production and more scientific and effective.

At the same time, in order to simulate the tension effect caused by the large-scale equipment of hydrolysis transformation in actual production, the inventor creatively designed a tension frame composed of springs, needle plates, support frames and needle plate fixing plates. The linkage relationship simulates the tension brought by large-scale equipment on the membrane, especially the design of the spring is more flexible, which can simulate the tension brought by different types of large-scale equipment in actual production.

The inventor also considers that in the process of the hydrolysis conversion reaction of the perfluorinated ion-exchange membrane, the ion-exchange membrane will swell and the size will become larger, so the pins and the needle-plate fixing plate used to fix the perfluorinated ion-exchange membrane will be fixed. The angle between them is designed to be greater than or equal to 45° and less than 90°; if it is not within this range, such as a right angle or an obtuse angle between the needle and the needle plate fixing plate, the ion exchange membrane is very easy to fall off during the reaction; but If the angle between the needle and the needle plate fixing plate is too small, it will be difficult for the membrane body to pass through the needle when fixing the ion exchange membrane, and the operation will be more difficult. On the contrary, it will easily cause artificial damage to the membrane and bring some unknown influencing factors. , which may lead to inaccuracies in the research parameters.

In combination with the above-mentioned design, the basic principle of using the device of the present invention to carry out research experiments is as follows: the perfluorinated ion exchange membrane is fixed on the needle plate fixing plate with the needles on the needle plate, and then the spring is used to connect the needle plate fixing plate and the support frame. At this time, the screws used to connect and fix the needle plate fixing plate in the horizontal direction and the vertical direction before are removed, so that the needle plate fixing plate drives the needle plate, and then drives the perfluorinated ion exchange membrane to receive the tension simulated by the spring, so as to simulate In the actual production process, the tension of the equipment to the membrane can be adjusted by adjusting the type of spring; fix the tension frame with the membrane on the plate frame, put the whole into the reaction tank filled with constant temperature solution, and turn on the circulation pump , so as to simulate the solution circulation system in the equipment tank in the actual production process. The above can complete the simulation of the hydrolysis process in actual production, and rely on this to complete the research work in the laboratory.

Compared with carrying out research experiments on large-scale production equipment, the advantages of the present invention are:

(1) save raw material cost, because hydrolysis reaction device self volume of the present invention is less, the required solution raw material of carrying out experimental research and perfluorinated ion-exchange membrane raw material consumption are less;

(2) The operation method is simple and easy, and there is no need to modify existing equipment and production lines, and it will not affect normal production. Although the reaction device of the present invention has no similarity with the actual production equipment in appearance, the perfluorinated ion exchange membrane samples tested can all be subjected to the effects similar to the production line equipment, such as tension and solution circulation force, etc. Make the final research results more realistic.

Description of drawings

Fig. 1 is a schematic diagram of the three-dimensional structure of an experimental perfluorinated ion exchange membrane hydrolysis conversion reaction device in a specific embodiment of the present invention.

Fig. 2 is a top view of an experimental perfluorinated ion exchange membrane hydrolysis conversion reaction device in a specific embodiment of the present invention.

Fig. 3 is a schematic perspective view of the three-dimensional structure of the reaction tank in the reaction device described in the specific embodiment of the present invention.

Fig. 4 is a front view of the reaction tank in the reaction device described in the specific embodiment of the present invention.

Fig. 5 is a left view of the reaction tank in the reaction device described in the specific embodiment of the present invention.

Fig. 6 is a top view of the reaction tank in the reaction device described in the specific embodiment of the present invention.

Fig. 7 is a schematic perspective view of the three-dimensional structure of the plate frame in the reaction device described in the specific embodiment of the present invention.

FIG. 8 is a partially enlarged view of the limiting groove in FIG. 7 .

Fig. 9 is a front view of the tray in the reaction device described in the specific embodiment of the present invention.

Fig. 10 is a left view of the tray in the reaction device described in the specific embodiment of the present invention.

Fig. 11 is a top view of the rack in the reaction device described in the specific embodiment of the present invention.

Fig. 12 is a schematic perspective view of the three-dimensional structure of the tension frame in the reaction device described in the specific embodiment of the present invention.

Fig. 13 is a front view of the tension frame in the reaction device described in the specific embodiment of the present invention.

Fig. 14 is a left view of the tension frame in the reaction device described in the specific embodiment of the present invention.

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

Fig. 16 is a front view of the support frame in the reaction device described in the specific embodiment of the present invention.

Fig. 17 is a left view of the support frame in the reaction device described in the specific embodiment of the present invention.

Fig. 18 is a schematic perspective view of the three-dimensional structure of the needle plate fixing plate in the vertical direction in the reaction device according to the specific embodiment of the present invention.

Fig. 19 is a front view of the needle plate fixing plate in the vertical direction in the reaction device according to the specific embodiment of the present invention.

Fig. 20 is a schematic perspective view of the three-dimensional structure of the needle plate fixing plate located in the horizontal direction in the reaction device in the specific embodiment of the present invention.

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

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

Among them, 1 is the electric heating tube, 2 is the thermocouple, 3 is the liquid circulation pipeline, 4 is the limit groove, 5 is the limit plate, 6 is the handle, 7 is the support frame, 8 is the needle plate fixing plate, and 9 is the Needle plate, 10 is positioning plate, and 11 is spring fixing hole, and 12 is needle plate fixing hole, and 13 is connecting hole, and 14 is plate frame.

Detailed ways

The technical solution of the present invention will be described in detail below in conjunction with the accompanying drawings. Many of the materials and procedures used in the experiments of this invention are well known in the art, but the invention is still described here in as much detail as possible.

The experimental perfluorinated ion exchange membrane hydrolysis conversion reaction device includes a circulation pump, a reaction tank, a plate frame 14 and a tension frame.

The rotating 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. The material of the circulating pump in the experimental perfluorinated ion exchange membrane hydrolysis conversion reaction device is PVDF, and its inner cavity is coated with PTFE.

The internal dimensions of the reaction tank height: length: width are 1-10:1-10:1-2.5; 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.

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

Wherein the electric heating tube 1 extends down to the bottom of the reaction tank along the inner wall of the narrow side 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 inner wall of the narrow side is ≤50 mm; 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 tube 1 forms the following view in the reaction tank: as shown in Figure 4, the electric heating tube 1 in the front view is similar to an "L" shape in the reaction tank; as shown in Figure 5, the electric heating tube 1 in the left view The tube 1 is similar to a "U" shape in the reaction tank; as shown in Figure 6, the electric heating tube 1 is similar to a "U" shape in the reaction tank in the top view. Among them, the distance between the outer walls of the "U"-shaped heating tube is ≤490mm.

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

The thermocouple 2 is installed at a position ≤ 1000 mm from the bottom of the reaction tank; preferably, the thermocouple 2 is installed at a position 50-800 mm away from the bottom of the reaction tank; more preferably, the thermocouple 2 is installed at a distance of 80 mm from the bottom of the reaction tank ~500mm position.

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

The plate frame 14 is a frame that matches the internal size of the reaction tank and is independent of the reaction tank, and can be flexibly placed and disassembled. The two sides of the frame are symmetrically provided with limiting grooves 4 for fixing the tension frame. Limiting grooves 4 are symmetrically defined as a group 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 limiting grooves 4 is equidistant; the grooves of the limiting grooves 4 The depth is 1-15mm, and the groove width is 1-15mm; the limiting groove 4 is provided with a limiting plate 5 for further fixing the position of the tension frame.

The above-mentioned 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;

A handle 6 is provided above the plate frame 14 to facilitate the loading and unloading of the plate frame 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 grade stainless steel or copper or iron-plated stainless steel.

The tension frame includes a spring, a needle plate 9 , a support frame 7 matching the size of the plate frame 14 and a needle plate fixing plate 8 placed in the support frame 7 .

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

A positioning plate 10 is arranged on the outer side of the supporting frame 7, and the positioning plate 10 corresponds to the plate frame limiting groove 4. The width of the positioning plate 10 is 1-15 mm, and the thickness is 1-15 mm. Four sides of the support frame 7 are provided with 1 to 20 spring fixing holes 11 .

There are 4 needle plate fixing plates 8 with a thickness of 1-50mm; the lengths of the two needle plate fixing plates 8 are both 115-915mm, and the two needle plate fixing plates 8 in this length range are used as the upper and lower horizontal sides; The total length of the spring fixing holes on the needle plate fixing plate 8 in the horizontal direction is 1-875 mm.

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 are used as the left and right vertical sides. The total length of the spring fixing holes on the needle plate fixing plate 8 in the vertical direction is 1-795mm.

The material of the needle plate fixing plate 8 can be selected from one of 304, 310, 310s, 316, 316L grade stainless steel or stainless steel with external electroplating of copper and iron.

One long edge of each needle plate fixing plate 8 is provided with 1 to 20 spring fixing holes 11, and when in use, the needle plate fixing plate 8 is connected with the support frame 7 by the spring and the spring fixing holes 11; The other long edge of the needle plate fixing plate 8 is provided with a needle plate fixing hole 12 for fixing the needle plate 9 .

Two short side ends of each needle plate fixing plate 8 are respectively provided with connecting holes 13 for fixedly connecting four needle plate fixing plates 8 . The horizontal and vertical needle plate fixing plates 8 are fixed to each other through the connecting holes 13 . When 4 needle plate fixing plates surrounded " back " font, spring fixing hole 11 was on the periphery of this " back " font, and needle plate fixing hole 12 was then on the inner periphery of this " back " font.

As shown in Figure 20-22, the needle plate fixing plate 8 located in the horizontal direction is in a “convex” shape as a whole, and the needle plate fixing plate 8 in the middle part with the spring fixing hole 11 is more fixed than the needle plate with connecting holes 13 on both sides. Plate 8 is higher than the thickness of a needle plate fixing plate.

The diameters of the above-mentioned spring fixing holes 11 are all 1-10 mm.

The needle plate 9 for fixing the perfluorinated ion exchange membrane includes a needle and a base. The length of the base is 20-880mm, and the width is 5-30mm; the length of the needles is 2-20mm; the number of needles contained in each needle board is 1-440; the needles are distributed on the base in 1-3 rows in the length direction. The material of the needle plate can be selected from one of 304, 310, 310s, 316, 316L grade stainless steel or stainless steel plated with copper and iron.

Wherein the angle between the needle and the needle plate fixing plate 8 is greater than or equal to 45° and less than 90°.

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 provided 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, 310, 310s, 316, 316L grade stainless steel.

Example 1

The experimental type perfluorinated ion exchange membrane hydrolysis transformation reaction device A, the material of the reaction tank is 310s stainless steel, the length of the reaction tank is 480mm, the width is 250mm, and the height is 450mm. The internal electric heating tube 1 is distributed in the shape of "U" in the reaction tank On the inner wall on one side of the width direction and the bottom of the reaction tank, the side overall presents an "L" shape, and two thermocouples 2 are respectively installed on the side walls in the width direction 100mm and 390mm away from the bottom of the reaction tank, and the direction is the same as the width of the reaction tank. The direction side wall is at an angle of 90°. Configure 25% NaOH+10% DMSO 28.5kg in the laboratory, add it to the reaction tank, adjust the temperature to 70°C, and turn on the PVDF material circulation pump coated with PTFE in the inner cavity to circulate the solution. The speed is 2750rpm, the flow rate is 15L/min, the power is 90W, the rated voltage is 220V, and the temperature is constant for half an hour.

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

Then fix the needle plate fixing plate placed in the horizontal direction and the needle plate fixing plate placed in the vertical direction by screws to form a rectangle.

Cut the hydrolyzed precursor chlor-alkali ion exchange membrane sampled from continuous production into samples with a length of 200mm and a width of 180mm, a total of 5 pieces, and fix them on the needle plate, and use a 10N 316 stainless steel spring to fix the needle plate 8 Four limits are connected to support frame 7 four limits, and each limit uses two springs; Remove the screw of the pin plate fixing plate of fixing horizontal direction and vertical direction, make film be subjected to the tension force effect from spring fully.

The support frames 7 with above-mentioned five groups of fixed membranes are inserted into the plate frame 14 along the limit groove 4, the plate frame 14 has a length of 400mm, a width of 220mm, a height (without the handle part) of 300mm, and the height of the handle 6 is 100mm, which can be inserted in total. 5 sets of supporting frames.

Put the above-mentioned plate frame 14 into the hydrolysis reaction tank as a whole, cover with a 310s stainless steel cover, and after 60 minutes of reaction, remove the plate frame 14, remove the hydrolyzed membrane, and wash the surface with water to obtain 5 sheets with ion exchange capacity. Chlor-alkali ion exchange membrane.

Example 2

The experimental perfluorinated ion exchange membrane hydrolysis conversion reaction device B is configured in the laboratory with 20% NaOH + 5% DMSO 18.3kg, added to the reaction tank, and the temperature is adjusted to 70°C. Others are the same as the reaction device A in Example 1, except that the length of the reaction tank of the reaction device B is 480 mm, the width is 160 mm, and the height is 450 mm.

Cut the hydrolyzed precursor chlor-alkali ion exchange membrane sampled from continuous production into samples with a length of 200mm and a width of 180mm, a total of 3 pieces, and fix them on the needle plate.

The above-mentioned three sets of supporting frames with fixed membranes are inserted into the plate frame along the limit groove. The plate frame 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 the handle 6 of 100 mm. 3 sets of supporting frames.

Put the above-mentioned plate frame 14 into the hydrolysis reaction tank as a whole, cover with a 310s stainless steel cover, after reacting for 60 minutes, remove the plate frame, remove the hydrolyzed membrane, and wash the surface with water to obtain 3 chlor-alkali with ion exchange capacity. ion exchange membrane.

Experimental example 1

1. The purpose of the experiment: to test the accuracy of the experimental perfluorinated ion exchange membrane hydrolysis conversion reaction device of the present invention simulating the large-scale hydrolysis equipment of the actual production line.

Two, the experimental method: first adopt the online production hydrolysis equipment to operate according to the hydrolysis treatment method in the embodiment 1 and the relevant hydrolysis conditions to obtain the online production sample 1; then the chlor-alkali ion exchange membrane obtained in the embodiment 1 and the online production sample 1 Carry out electrolysis test respectively, and compare the test results.

3. Experimental conclusions: The experimental results are shown in Table 1.

Table 1 Example 1 gained chlor-alkali ion exchange membrane and online production sample 1 performance comparison

It can be seen from the comparison in Table 1 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 average voltage of the sample 1 produced on-line is 2.987V, and the standard deviation is 0.002. The stability of the two is equivalent, and the average difference is only 0.009V. It is considered that the performance of the membrane obtained by the method of the present invention is equivalent to that of the online production membrane. It can be seen that, by carrying out the membrane hydrolysis transformation research experiment by the experimental type perfluorinated ion exchange membrane hydrolysis transformation reaction device described in the present invention, the optimized data obtained can be directly applied to the large-scale hydrolysis production equipment on the continuous production line, without further Conduct pilot tests, etc.

Experimental example 2

1. The purpose of the experiment: to test the accuracy of the experimental perfluorinated ion exchange membrane hydrolysis conversion reaction device of the present invention simulating the large-scale hydrolysis equipment of the actual production line.

Two, the experimental method: first adopt the online production hydrolysis equipment to operate according to the hydrolysis treatment method in the embodiment 2 and the relevant hydrolysis conditions to obtain the online production sample 2; 2 Carry out electrolysis test respectively, and compare the test results.

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

Table 2 Example 2 gained chlor-alkali ion exchange membrane and online production sample 2 performance comparison

It can be seen from the comparison in Table 2 that the average electrolysis voltage of the ion exchange membrane prepared in Example 2 is 3.027V, and the standard deviation is 0.005; the average voltage of the online production sample 2 is 3.038V, and the standard deviation is 0.003. The stability of the two is equivalent, and the average difference is only 0.011V. It is considered that the performance of the membrane obtained by the method of the present invention is equivalent to that of the online production membrane.

Claims (10)

1. An experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device is characterized by comprising a circulating pump, a reaction tank, a plate frame and a tension frame; 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; a heating part, a temperature measuring part and a liquid circulating pipeline are arranged in the reaction tank, wherein the liquid circulating pipeline is connected with a circulating pump; the plate frame is a detachable frame matched with the inner size of the reaction tank, and limiting grooves for fixing the tension frame are symmetrically arranged in two sides of the frame; the tension bracket comprises a spring, a needle plate, a supporting frame matched with the plate frame in size and a needle plate fixing plate arranged in the supporting frame; a positioning plate is arranged on the outer side of the supporting frame and corresponds to the plate frame limiting groove; the four edges of the supporting 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 device is used, the needle plate fixing plates are connected with the supporting 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 an included angle between the needle and the needle plate fixing plate is more than or equal to 45 degrees and less than 90 degrees; a needle plate fixing hole is arranged on the base of the needle plate and corresponds to the needle plate fixing hole arranged on the needle plate fixing plate.

2. The experimental perfluorinated ion exchange membrane hydrolysis-transformation reaction device of claim 1, wherein the circulating pump is made of PVDF, and the inner cavity of the circulating pump is coated with PTFE; the heating component adopts an electric heating pipe; the temperature measuring component adopts a thermocouple.

3. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device of claim 2, wherein the electric heating tube 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 pipe and the inner wall of the narrow side is less than or equal to 50mm; the outer diameter of the electric heating tube is 5-20 mm, and the inner diameter is 3-18 mm; at least 1 thermocouple is arranged at the position which is less than or equal to 1000mm away from the bottom of the reaction tank;

preferably, the thermocouple is arranged at a position 50-800 mm away from the bottom of the reaction tank;

more preferably, the thermocouple is installed at a position 80 to 500mm from the bottom of the reaction tank.

4. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device of claim 1, wherein the liquid inlet of the liquid circulation 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 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 liquid circulation pipeline, which is positioned outside the reaction tank, is 5-20 mm, the inner diameter of the part of the liquid circulation pipeline is 3-18 mm, and the part of the liquid circulation pipeline is connected with a circulating pump through a hose with the outer diameter of 3-18 mm and the inner diameter of 1-16 mm.

5. The apparatus for the hydrolysis-conversion reaction of an experimental perfluorinated ion exchange membrane according to claim 1, wherein the height of the internal dimension of the reaction tank is as follows: length: the width is 1-10;

preferably, the reaction tank has an inner dimension of 200 to 1000mm in height, 200 to 1000mm in length, and 100 to 500mm in width.

6. The experimental perfluorinated ion exchange membrane hydrolysis-transformation reaction device of claim 1, wherein the limiting grooves are symmetrically arranged at two sides into one group, and the total number of the groups is 1-10; each group of adjacent limiting grooves are equidistant; the groove depth of the limiting groove is 1-15 mm, and the groove width is 1-15 mm; a limiting plate is arranged in the limiting groove; the width of the positioning plate is 1-15 mm, and the thickness of the positioning plate is 1-15 mm.

7. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device as claimed in claim 1, wherein the length of the plate frame 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;

preferably, a handle is arranged above the plate frame, wherein the height of the handle is 50-200 mm, and the width of the handle is 50-200 mm.

8. The experimental perfluorinated ion exchange membrane hydrolysis-transformation reaction device as claimed in claim 1, wherein the support frame is square, the width of the outer side of the support frame 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 support frame is 100-840 mm, and the length of the inner side is 120-920 mm.

9. The experimental perfluorinated ion exchange membrane hydrolysis transformation reaction device of claim 1, wherein the thickness of the 4 needle plate fixing plates is 1-50 mm; wherein the length of each of the 2 needle plate fixing plates is 115-915 mm, and the length of each of the other 2 needle plate fixing plates is 95-835 mm;

the number of the spring fixing holes arranged on each edge of the supporting frame and the number of the spring fixing holes arranged on the needle plate fixing plate are 1-20; the aperture of each spring fixing hole is 1-10 mm;

the number of the needle plate fixing holes is 2-10; the tension range of the spring is 0.1-100N.

10. The experimental perfluorinated ion exchange membrane hydrolysis-transformation reaction device of claim 1, wherein the base has a length of 20-880 mm and a width of 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 on the base in 1-3 rows.

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