CN113856601A - Preparation method of high-concentration perfluorosulfonic acid solution - Google Patents
Preparation method of high-concentration perfluorosulfonic acid solution Download PDFInfo
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- CN113856601A CN113856601A CN202111300222.1A CN202111300222A CN113856601A CN 113856601 A CN113856601 A CN 113856601A CN 202111300222 A CN202111300222 A CN 202111300222A CN 113856601 A CN113856601 A CN 113856601A
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- heating tank
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- acid solution
- perfluorosulfonic acid
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- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 154
- 239000007788 liquid Substances 0.000 claims abstract description 47
- 239000011347 resin Substances 0.000 claims abstract description 41
- 229920005989 resin Polymers 0.000 claims abstract description 41
- 239000002904 solvent Substances 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 30
- 150000003460 sulfonic acids Chemical class 0.000 claims abstract description 27
- 239000011261 inert gas Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims description 35
- 230000007246 mechanism Effects 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 10
- 238000005192 partition Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000005389 magnetism Effects 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000009835 boiling Methods 0.000 abstract description 8
- 238000005406 washing Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 40
- 239000003014 ion exchange membrane Substances 0.000 description 7
- 230000017525 heat dissipation Effects 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical group [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N dimethyl sulfoxide Natural products CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005373 pervaporation Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 210000001114 tooth apex Anatomy 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention relates to the technical field of perfluorinated sulfonic acid solution, in particular to a preparation method of high-concentration perfluorinated sulfonic acid solution, which comprises the steps of preparing the high-concentration perfluorinated sulfonic acid solution by a reaction kettle, wherein the reaction kettle comprises a heating tank for heating the prepared solution; and a magnet disposed outside the heating tank; the magnet is arranged in the heating tank and is in magnetic connection with the magnet; and a first servo motor driving the magnet to rotate, the preparation method comprising the steps of: injecting perfluorinated sulfonic acid resin and a high-boiling-point solvent into a closed heating tank; replacing the gas inside the heating tank with inert gas; first servo motor drive magnet is rotatory, and it is rotatory that magnet passes through the magnetic drive bar magnet, and the bar magnet drives the stirring leaf and stirs the mixed liquid of type perfluorosulfonic acid resin and high boiling point solvent, through the setting of this equipment, has realized the purpose that type perfluorosulfonic acid resin and high boiling point solvent high temperature mix, and the inside washing of heating tank can be convenient for to this structure.
Description
Technical Field
The invention relates to the technical field of perfluorinated sulfonic acid solution, and particularly relates to a preparation method of high-concentration perfluorinated sulfonic acid solution.
Background
The world is facing to many problems such as energy shortage, environmental pollution, global climate change and the like, in order to protect the environment on which human beings rely for survival and realize the continuous development of global economy, the development of clean, efficient, safe and sustainable energy is urgent, and the primary application of the perfluorinated sulfonic acid ion exchange membrane fuel cell is to replace an automobile engine as a new traffic energy conversion device, so that the demand is huge. The ion exchange membrane fuel cell uses hydrogen and oxygen as fuel and oxygen source respectively, and is a technology which is preferred in the world at present and can synthesize pure water from hydrogen and oxygen in air and release electric energy. The ion exchange membrane technology has great demand in the chlor-alkali industry, so that the localization of the ion membrane is realized, and China occupies a place in the chlor-alkali industry in the world, which is urgent and necessary. In addition, the perfluorinated ion exchange membrane is widely applied to many fields such as pervaporation, gas separation, photocatalysis and the like, and various excellent performances of the perfluorinated ion exchange membrane are widely regarded at home and abroad, so that many companies and scientific research institutions are actively exploring the perfluorinated ion exchange membrane, the application range of the perfluorinated ion exchange membrane is continuously expanded, and the development prospect is very wide. The preparation of perfluorosulfonic acid proton exchange membranes has attracted the attention of researchers all over the world, but the key point is to prepare a qualified perfluorosulfonic acid resin solution.
Chinese patent: CN201310166887.7 provides a preparation method of perfluorosulfonic acid resin solution, and provides a preparation method of perfluorosulfonic acid resin solution with simple process and convenient operation. The method comprises the following steps: a) adding 4-35 wt% ROH solution into perfluorinated sulfonic acid resin containing sulfonic acid functional group, and soaking for 2-36 hours at 12-99 ℃; b) placing the perfluorinated sulfonic acid resin soaked in the step a) into a container, washing the perfluorinated sulfonic acid resin with pure water until the pH value is 7, washing the perfluorinated sulfonic acid resin at the temperature of 40-100 ℃, and drying the perfluorinated sulfonic acid resin at the temperature of 25-120 ℃ to obtain R-type perfluorinated sulfonic acid resin; c) placing the R-type perfluorosulfonic acid resin treated in the step b) into a container, and adding a high-boiling-point solvent. The method has the advantages of simple process, strong repeatability, capability of saving a large amount of manpower, material resources and time and important industrial significance.
In this patent, the third step for the preparation of perfluorosulfonic acid resin solution: and (2) placing the treated R-type perfluorosulfonic acid resin in a container, adding a high-boiling-point solvent, magnetically stirring under the protection of inert gas, controlling the temperature to be 130-280 ℃, keeping for 4-30 hours, stopping heating and stirring, and naturally cooling at room temperature to obtain an R-type perfluorosulfonic acid resin solution.
However, there is no apparatus for the third step preparation, so that a method for preparing a high-concentration perfluorosulfonic acid solution is required to solve the above problems.
Disclosure of Invention
To solve the above technical problems.
The application provides a preparation method of a high-concentration perfluorinated sulfonic acid solution, which is characterized in that the high-concentration perfluorinated sulfonic acid solution is prepared through a reaction kettle, and the reaction kettle comprises a heating tank for heating the preparation solution; and a magnet disposed outside the heating tank; the magnet is arranged in the heating tank and is in magnetic connection with the magnet; the stirring blade is arranged at the top of the magnetic rod, the hemispherical bearing part is arranged at the bottom of the magnetic rod, and the stirring blade and the bearing part are nonmagnetic; the preparation method comprises the following steps:
injecting R-type perfluorinated sulfonic acid resin and a high-boiling-point solvent into a closed heating tank;
replacing the gas inside the heating tank with inert gas;
the first servo motor drives the magnet to rotate, the magnet drives the magnetic rod to rotate through magnetic force, and the magnetic rod drives the stirring blade to stir the mixed liquid of the R-type perfluorinated sulfonic acid resin and the high-boiling-point solvent.
Preferably, the reaction kettle further comprises a sealing mechanism, the top of the heating tank is provided with a feed inlet, the sealing mechanism is arranged at the feed inlet of the heating tank, and the preparation method further comprises the following steps: the sealing mechanism opens the feed inlet at the top of the heating tank; pouring the treated R-type perfluorinated sulfonic acid resin into a heating tank; the sealing mechanism closes the feed inlet at the top of the heating tank.
Preferably, the side wall of the heating tank is provided with a liquid inlet valve, the liquid inlet valve is positioned above the heating tank, and the preparation method further comprises the following steps: and opening the liquid inlet valve, injecting the high-boiling-point solvent into the heating tank through the liquid inlet valve, and then closing the liquid inlet valve. Preferably, the top of the sealing mechanism is provided with an air inlet valve and an air outlet valve, and the preparation method further comprises the following steps: and opening the air inlet valve and the air outlet valve, injecting inert gas into the heating tank through the air inlet valve, filling the inert gas into the heating tank, and closing the air inlet valve and the air outlet valve.
Preferably, the heating tank comprises an inner container for containing the solution; the heating wire is wound outside the inner container; the heat preservation layer is used for preventing heat generated by the heating wire from leaking outside, wraps the outside of the heating wire and is fixedly connected with the inner container, and the preparation method further comprises the following steps; the heating tank starts to work, and the heating wire is electrified to heat; the heating wire heats the mixture in the inner container through the inner container; controlling the heating temperature between the centigrade degree and the centigrade degree, and keeping for hours to hours; in the heating process, the first servo motor drives the magnet to rotate, the magnet drives the magnetic rod to rotate through magnetic force, and the magnetic rod drives the stirring blade to stir the mixed liquid of the R-type perfluorosulfonic acid resin and the high-boiling-point solvent until the stirring is stopped after the heating is stopped.
Preferably, the side wall of the heating tank is provided with a liquid outlet valve, and the liquid outlet valve is positioned below the heating tank; opening the sealing mechanism to cool the mixture in the heating tank at room temperature to obtain a high-concentration perfluorosulfonic acid solution; and opening the liquid outlet valve to discharge the cooled high-concentration perfluorosulfonic acid solution.
Preferably, the reaction kettle further comprises a pump, the input end of the pump is connected with the liquid outlet valve through a pipeline, and the preparation method further comprises the following steps; and opening the pump, and pumping out the cooled high-concentration perfluorosulfonic acid solution in the heating tank through the liquid outlet valve.
Preferably, the sealing mechanism comprises a top cover for closing the feed inlet of the heating tank; the clamping ring is arranged outside the heating tank, a threaded rod and a guide rod are symmetrically arranged on the clamping ring, the threaded rod is rotatably connected with the clamping ring, the guide rod is fixedly connected with the clamping ring, the threaded rod is in threaded connection with the top cover, and the guide rod is in sliding connection with the top cover; and the second servo motor is arranged on the clamping ring, and the output end of the second servo motor is connected with the threaded rod.
Preferably, the bottom of top cap is equipped with the baffle, and admission valve and air outlet valve all set up in the top of top cap, and admission valve and air outlet valve are located the both sides of baffle respectively.
Preferably, sealing mechanism still includes door plant and unipolar cylinder, is equipped with the dog-house on the top cap, and the door plant is in dog-house department to one side and the top cap of door plant are articulated, and the stiff end and the top cap top of unipolar cylinder are articulated, and the output and the door plant of unipolar cylinder are articulated.
Compared with the prior art, the invention has the beneficial effects that:
1. this application has realized the purpose of R type perfluorosulfonic acid resin and high boiling point solvent high temperature mixture through heating jar, magnet, bar magnet, stirring leaf, bearing part and first servo motor's setting, and the inside washing of heating jar can be convenient for to this structure.
2. This application can provide the special line that high boiling point solvent got into the heating jar through the setting of feed liquor valve, improves production efficiency.
3. This application can make inert gas can be full of the inside of heating jar through the setting of top cap, baffle, admission valve and air outlet valve, avoids the air to remain.
4. This application can carry out inside seal and open the heat dissipation to the heating jar through top cap, rand, threaded rod, guide bar and second servo motor's setting.
5. This application can only open the dog-house on the top cap at the feed inlet that opens that need not to open the whole feed inlets of heating jar through the setting of door plant and unipolar cylinder, has avoided the whole time and the energy that consume of opening of top cap.
Drawings
FIG. 1 is a first perspective view of the present invention;
FIG. 2 is a schematic perspective view of the present invention;
FIG. 3 is a front view of the present invention;
FIG. 4 is a side view of the present invention;
FIG. 5 is a sectional view taken along line A-A of FIG. 4;
FIG. 6 is a schematic perspective view of a heating tank of the present invention;
FIG. 7 is a side view of a heating tank of the present invention;
FIG. 8 is a sectional view taken along line B-B of FIG. 7;
FIG. 9 is a schematic perspective view of a heating tank, a liquid inlet valve and a liquid outlet valve according to the present invention;
FIG. 10 is a front view of the heating tank and sealing mechanism of the present invention;
FIG. 11 is a schematic perspective view of a heating tank and sealing mechanism of the present invention;
FIG. 12 is an enlarged view at C of FIG. 11;
FIG. 13 is a side view of the heating tank, air inlet valve, air outlet valve, top cover and baffle of the present invention;
FIG. 14 is a cross-sectional view taken along line D-D of FIG. 13;
FIG. 15 is a front view of the heating tank, effluent valve and pump of the present invention;
the reference numbers in the figures are:
1-heating the tank; 1 a-inner container; 1 b-heating wires; 1 c-a heat-insulating layer;
2-a liquid inlet valve;
3-a liquid outlet valve;
4 a-a magnet; 4 b-a magnetic bar; 4b 1-stirring blade; 4b 2-carrier part; 4 c-a first servomotor;
5-a sealing mechanism; 5 a-a top cover; 5a 1-baffle; 5 b-a collar; 5b 1-threaded rod; 5b 2-guide bar; 5 c-a second servomotor; 5 d-door panel; 5 e-single axis cylinder;
6-an air inlet valve;
7-an air outlet valve;
8-pump.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
As shown in fig. 1, fig. 2, fig. 3, fig. 4 and fig. 5, the following preferred technical solutions are provided:
a preparation method of a high-concentration perfluorinated sulfonic acid solution comprises the steps of preparing the high-concentration perfluorinated sulfonic acid solution through a reaction kettle, wherein the reaction kettle comprises a heating tank 1 for heating the preparation solution; and a magnet 4a provided outside the heating tank 1; and a magnetic rod 4b arranged inside the heating tank 1, the magnet 4a being magnetically connected with the magnetic rod 4 b; the first servo motor 4c drives the magnet 4a to rotate, the top of the magnetic rod 4b is provided with a stirring blade 4b1, the bottom of the magnetic rod 4b is provided with a hemispherical bearing part 4b2, and the stirring blade 4b1 and the bearing part 4b2 are nonmagnetic; the preparation method comprises the following steps:
injecting R-type perfluorinated sulfonic acid resin and a high-boiling-point solvent into the sealed heating tank 1;
replacing the gas inside the heating tank 1 with inert gas;
the first servo motor 4c drives the magnet 4a to rotate, the magnet 4a drives the magnetic rod 4b to rotate through magnetic force, and the magnetic rod 4b drives the stirring blade 4b1 to stir the mixed liquid of the R-type perfluorosulfonic acid resin and the high-boiling-point solvent;
specifically, in order to solve the technical problem of the high-concentration perfluorosulfonic acid solution preparation device without needles, a worker injects an R-type perfluorosulfonic acid resin and a high-boiling-point solvent into the heating tank 1, and after the internal gas of the heating tank 1 is replaced by inert gas, in order to ensure that the R-type perfluorosulfonic acid resin and the high-boiling-point solvent are fully mixed, a stirring blade 4b1 is added on the top of the magnetic rod 4b, the stirring blade 4b1 is in a spiral blade shape, so that the situation that only the magnetic rod 4b rotates to drive liquid to flow and mix is avoided, the mixing mode is insufficient in strength, the stirring blade 4b1 is arranged above the magnetic rod 4b, so that the gravity center is unstable, the gravity center is limited by a hemispherical bearing part 4b2 arranged at the bottom of the magnetic rod 4b, the bearing part 4b2 has a certain weight and has the effect of a tumbler base, and the magnets 4a are driven by a first servo motor 4c to rotate, The principle of opposite attraction is that magnetic rods 4b with magnetism placed in a container are pushed by a magnetic field to perform circumferential operation, and the inside of the heating tank 1 can be cleaned conveniently in a magnetic stirring mode.
As shown in fig. 2 and 3, the following preferred solutions are provided:
the reaction kettle further comprises a sealing mechanism 5, a feed inlet is formed in the top of the heating tank 1, the sealing mechanism 5 is arranged at the feed inlet of the heating tank 1, and the preparation method further comprises the following steps:
the sealing mechanism 5 opens the feed inlet at the top of the heating tank 1;
pouring the treated R-type perfluorinated sulfonic acid resin into the heating tank 1;
the sealing mechanism 5 closes the feed inlet at the top of the heating tank 1;
specifically, in order to solve the technical problem of forming a closed space in the heating tank 1, the R-type perfluorosulfonic acid resin and the high-boiling point solvent need to be heated at a high temperature and assisted by inert gas, so that the feed inlet needs to be closed in time by the sealing mechanism 5 after the R-type perfluorosulfonic acid resin and the high-boiling point solvent enter the heating tank 1, and the loss and heat dissipation of the inert gas are avoided.
As shown in fig. 9, the following preferred technical solutions are provided:
the side wall of the heating tank 1 is provided with a liquid inlet valve 2, the liquid inlet valve 2 is positioned above the heating tank 1, and the preparation method further comprises the following steps:
opening the liquid inlet valve 2, injecting a high-boiling-point solvent into the heating tank 1 through the liquid inlet valve 2, and then closing the liquid inlet valve 2;
specifically, in order to solve the technical problem that no special line is used for injecting the high-boiling-point solvent, the high-boiling-point solvent is required to be injected into the heating tank 1 through the liquid inlet formed by the liquid inlet valve 2, the high-boiling-point solvent can be conveniently and quickly injected into the heating tank, the position of the liquid inlet valve 2 cannot be relatively low, the liquid inlet is prevented from being blocked by the R-type perfluorinated sulfonic acid resin, and the high-boiling-point solvent is dimethyl sulfoxide, ethylene glycol, pyrrolidone or dimethylformamide.
As shown in fig. 14, the following preferred technical solutions are provided:
the top of the sealing mechanism 5 is provided with an air inlet valve 6 and an air outlet valve 7, and the preparation method further comprises the following steps:
opening an air inlet valve 6 and an air outlet valve 7, injecting inert gas into the heating tank 1 through the air inlet valve 6, and then closing the air inlet valve 6 and the air outlet valve 7;
specifically, in order to solve the technical problem of replacing the air inside the heating tank 1 with inert gas, the air inlet valve 6 provides an injection point of the inert gas through the arrangement of the air inlet valve 6 and the air outlet valve 7, and the air inside the heating tank 1 is discharged from the air outlet valve 7 when being extruded by new entering air in the injection process of the air inlet valve 6.
As shown in fig. 6, 7 and 8, the following preferred technical solutions are provided:
the heating tank 1 comprises an inner container 1a for containing solution; the heating wire 1b is used for heating the inner container 1a, and the heating wire 1b is wound outside the inner container 1 a; the heat insulation layer 1c is used for preventing heat generated by the heating wire 1b from leaking outside, and the heat insulation layer 1c is wrapped outside the heating wire 1b and is fixedly connected with the inner container 1 a;
the heating tank 1 starts to work, and the heating wire 1b is electrified to heat;
the heating wire 1b heats the mixture in the inner container 1 a;
controlling the heating temperature to be 130-280 ℃, and keeping for 4-30 hours;
in the heating process, the first servo motor 4c drives the magnet 4a to rotate, the magnet 4a drives the magnetic rod 4b to rotate through magnetic force, and the magnetic rod 4b drives the stirring blade 4b1 to stir the mixed liquid of the R-type perfluorosulfonic acid resin and the high-boiling-point solvent until the heating is stopped;
specifically, in order to solve the technical problem to R type perfluorosulfonic acid resin and high boiling point solvent heating, when R type perfluorosulfonic acid resin and high boiling point solvent are in inner bag 1a inside and pour into inert gas and the apical foramen is sealed, heater strip 1b circular telegram heats inner bag 1a, inner bag 1a conducts the mixture to its inside with the heat, through installing in temperature sensor, temperature sensor's receiving terminal is in inner bag 1 a's inside, detect the inside temperature of inner bag 1a, heat preservation 1c is used for preventing heater strip 1b heat from giving off and protection staff.
As shown in fig. 9, the following preferred technical solutions are provided:
the side wall of the heating tank 1 is provided with a liquid outlet valve 3, the liquid outlet valve 3 is positioned below the heating tank 1, and the preparation method further comprises the following steps;
opening the sealing mechanism 5 to cool the mixture in the heating tank 1 at room temperature to obtain a high-concentration perfluorosulfonic acid solution;
opening the liquid outlet valve 3 to discharge the cooled high-concentration perfluorosulfonic acid solution;
specifically, in order to solve the technical problem of discharging the finished product of the high-concentration perfluorosulfonic acid solution, the feed inlet of the heating tank 1 is opened through the sealing mechanism 5, so that the internal mixture is cooled at room temperature to the high-concentration perfluorosulfonic acid solution, then the sealing mechanism 5 is opened and is positioned below the side wall of the heating tank 1, and the high-concentration perfluorosulfonic acid solution can be discharged from the sealing mechanism 5 under the action of gravity.
As shown in fig. 15, the following preferred technical solutions are provided:
the reaction kettle also comprises a pump 8, the input end of the pump 8 is connected with the liquid outlet valve 3 through a pipeline, and the preparation method also comprises the following steps;
the pump 8 is started, and the pump 8 pumps out the cooled high-concentration perfluorosulfonic acid solution in the heating tank 1 through the liquid outlet valve 3;
specifically, in order to solve the technical problem that the high-concentration perfluorosulfonic acid solution is discharged slowly, the pump 8 is installed, and after the liquid outlet valve 3 is opened, the high-concentration perfluorosulfonic acid solution in the heating tank 1 is rapidly pumped out under the action of the pump 8, so that the production efficiency is improved.
As shown in fig. 10 and 11, the following preferred technical solutions are provided:
the sealing mechanism 5 comprises a top cover 5a for closing the feed inlet of the heating tank 1; and
the clamping ring 5b is arranged outside the heating tank 1, the clamping ring 5b is symmetrically provided with a threaded rod 5b1 and a guide rod 5b2, the threaded rod 5b1 is rotatably connected with the clamping ring 5b, the guide rod 5b2 is fixedly connected with the clamping ring 5b, the threaded rod 5b1 is in threaded connection with the top cover 5a, and the guide rod 5b2 is in sliding connection with the top cover 5 a; and
the second servo motor 5c is arranged on the collar 5b, and the output end of the second servo motor 5c is connected with the threaded rod 5b 1;
specifically, in order to solve the technical problems of feeding, sealing and heat dissipation of the heating tank 1, when the R-type perfluorosulfonic acid resin and the high-boiling-point solvent are in the heating tank 1, the sealing mechanism 5 starts to work, the output end of the second servo motor 5c can drive the threaded rod 5b1 to rotate, the threaded rod 5b1 drives the top cover 5a to descend along the guide rod 5b2, the bottom of the top cover 5a is provided with a sealing ring, the top cover 5a descends to the feed inlet of the heating tank 1 to seal the feed inlet, and the clamping ring 5b is used for fixing and supporting.
As shown in fig. 13 and 14, the following preferred technical solutions are provided:
the air inlet valve is characterized in that a partition plate 5a1 is arranged at the bottom of the top cover 5a, the air inlet valve 6 and the air outlet valve 7 are both arranged at the top of the top cover 5a, and the air inlet valve 6 and the air outlet valve 7 are respectively positioned at two sides of the partition plate 5a 1. (ii) a
Specifically, in order to solve the technical problem that the heating tank 1 is difficult to be filled with inert gas, when the top cover 5a is closed at the feed inlet of the heating tank 1, the partition plate 5a1 extends to the half of the interior of the heating tank 1 and divides the interior of the heating tank 1 to form an inert gas injection route, the inert gas is injected into the heating tank 1 through the air inlet valve 6, the inert gas is pushed into the heating tank 1 in a U shape to be discharged from the air outlet valve 7 through the action of the partition plate 5a1, and after the air in the heating tank 1 is discharged, the inert gas occupies the interior of the heating tank 1.
As shown in fig. 12, the following preferred technical solutions are provided:
the sealing mechanism 5 further comprises a door plate 5d and a single-shaft cylinder 5e, a feeding port is formed in the top cover 5a, the door plate 5d is located at the feeding port, one side of the door plate 5d is hinged to the top cover 5a, the fixed end of the single-shaft cylinder 5e is hinged to the top of the top cover 5a, and the output end of the single-shaft cylinder 5e is hinged to the door plate 5 d;
concretely, in order to solve the technical problem of the quick feeding of R type perfluorosulfonic acid resin, when need not that top cap 5a is whole to be opened, can drop into heating tank 1 with R type perfluorosulfonic acid resin inside, the output of unipolar cylinder 5e contracts and pulls door plant 5d and opens, then drops into heating tank 1's inside with R type perfluorosulfonic acid resin, then unipolar cylinder 5e promotes door plant 5d and closes the dog-house, top cap 5a shifts up again and opens the whole feed inlet in heating tank 1 top when needs dispel the heat.
The purpose of mixing R-type perfluorosulfonic acid resin and high-boiling-point solvent at high temperature is achieved through the arrangement of the heating tank 1, the magnet 4a, the magnetic rod 4b, the stirring blade 4b1, the bearing part 4b2 and the first servo motor 4c, the structure can facilitate the cleaning of the interior of the heating tank 1, the special line for the high-boiling-point solvent to enter the heating tank 1 can be provided through the arrangement of the liquid inlet valve 2, the production efficiency is improved, the inert gas can be filled in the heating tank 1 through the arrangement of the top cover 5a, the partition plate 5a1, the air inlet valve 6 and the air outlet valve 7, the air residue is avoided, the internal sealing and the opening heat dissipation can be carried out on the heating tank 1 through the arrangement of the top cover 5a, the clamping ring 5b, the threaded rod 5b1, the guide rod 5b2 and the second servo motor 5c, the opening of the feeding channel of all feed inlets of the heating tank 1 can be opened through the arrangement of the door plate 5d and the single-axis cylinder 5e, only the feeding port on the top cover 5a is opened, so that the time and energy consumption caused by the integral opening of the top cover 5a are avoided.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A preparation method of a high-concentration perfluorinated sulfonic acid solution comprises the steps of preparing the high-concentration perfluorinated sulfonic acid solution through a reaction kettle, wherein the reaction kettle comprises a heating tank (1) for heating the preparation solution; and a magnet (4a) provided outside the heating tank (1); and a magnetic rod (4b) arranged inside the heating tank (1), wherein the magnet (4a) is in magnetic connection with the magnetic rod (4 b); the first servo motor (4c) is used for driving the magnet (4a) to rotate, and is characterized in that the top of the magnetic rod (4b) is provided with a stirring blade (4b1), the bottom of the magnetic rod (4b) is provided with a hemispherical bearing part (4b2), and the stirring blade (4b1) and the bearing part (4b2) have no magnetism; the preparation method comprises the following steps:
injecting R-type perfluorinated sulfonic acid resin and a high-boiling-point solvent into a closed heating tank (1);
replacing the gas inside the heating tank (1) with inert gas;
the first servo motor (4c) drives the magnet (4a) to rotate, the magnet (4a) drives the magnetic rod (4b) to rotate through magnetic force, and the magnetic rod (4b) drives the stirring blade (4b1) to stir the mixed liquid of the R-type perfluorosulfonic acid resin and the high-boiling-point solvent.
2. The method for preparing the high-concentration perfluorosulfonic acid solution according to claim 1, wherein the reaction kettle further comprises a sealing mechanism (5), the top of the heating tank (1) is provided with a feeding port, the sealing mechanism (5) is arranged at the feeding port of the heating tank (1), and the method further comprises the following steps:
the sealing mechanism (5) opens a feed inlet at the top of the heating tank (1);
pouring the treated R-type perfluorinated sulfonic acid resin into the heating tank (1);
the sealing mechanism (5) closes the feed inlet at the top of the heating tank (1).
3. The method for preparing the high-concentration perfluorosulfonic acid solution according to claim 1, wherein the heating tank (1) is provided with a liquid inlet valve (2) on the side wall, and the liquid inlet valve (2) is positioned above the heating tank (1), and the method further comprises the following steps:
and opening the liquid inlet valve (2), injecting the high-boiling-point solvent into the heating tank (1) through the liquid inlet valve (2), and then closing the liquid inlet valve (2).
4. The method for preparing a high-concentration perfluorosulfonic acid solution according to claim 1, wherein the sealing mechanism (5) is provided with an air inlet valve (6) and an air outlet valve (7) at the top, and the method further comprises the steps of:
and opening the air inlet valve (6) and the air outlet valve (7), injecting inert gas into the heating tank (1) through the air inlet valve (6), and closing the air inlet valve (6) and the air outlet valve (7).
5. The method for preparing a highly concentrated perfluorosulfonic acid solution according to claim 1, wherein the heating tank (1) comprises a tank (1a) for holding the solution; and a heating wire (1b) for heating the inner container (1a), the heating wire (1b) being wound around the outside of the inner container (1 a); the heat insulation layer (1c) is used for preventing heat generated by the heating wire (1b) from leaking outside, the heat insulation layer (1c) is wrapped outside the heating wire (1b) and is fixedly connected with the inner container (1a), and the preparation method further comprises the following steps;
the heating tank (1) starts to work, and the heating wire (1b) is electrified to heat;
the heating wire (1b) heats the mixture in the inner container (1a) through the inner container;
controlling the heating temperature to be 130-280 ℃, and keeping for 4-30 hours;
in the heating process, the first servo motor (4c) drives the magnet (4a) to rotate, the magnet (4a) drives the magnetic rod (4b) to rotate through magnetic force, and the magnetic rod (4b) drives the stirring blade (4b1) to stir the mixed liquid of the R-type perfluorosulfonic acid resin and the high-boiling-point solvent until the stirring is stopped after the heating is stopped.
6. The method for preparing the high-concentration perfluorosulfonic acid solution according to claim 1, wherein the heating tank (1) is provided with a liquid outlet valve (3) on the side wall, and the liquid outlet valve (3) is positioned below the heating tank (1), and the method further comprises the following steps;
opening the sealing mechanism (5) to cool the mixture in the heating tank (1) at room temperature to obtain a high-concentration perfluorosulfonic acid solution;
and opening the liquid outlet valve (3) to discharge the cooled high-concentration perfluorosulfonic acid solution.
7. The method for preparing a high-concentration perfluorosulfonic acid solution according to claim 6, wherein the reaction vessel further comprises a pump (8), and the input end of the pump (8) is connected to the outlet valve (3) through a pipe, and the method further comprises the steps of;
and (3) opening the pump (8), and pumping out the cooled high-concentration perfluorosulfonic acid solution in the heating tank (1) by the pump (8) through the liquid outlet valve (3).
8. The method for producing a highly concentrated perfluorosulfonic acid solution according to claim 2, wherein the sealing means (5) comprises a top cover (5a) for closing the feed port of the heating tank (1); and
the clamping ring (5b), the clamping ring (5b) is arranged outside the heating tank (1), a threaded rod (5b1) and a guide rod (5b2) are symmetrically arranged on the clamping ring (5b), the threaded rod (5b1) is rotatably connected with the clamping ring (5b), the guide rod (5b2) is fixedly connected with the clamping ring (5b), the threaded rod (5b1) is in threaded connection with the top cover (5a), and the guide rod (5b2) is in sliding connection with the top cover (5 a); and
and the second servo motor (5c), the second servo motor (5c) is arranged on the clamping ring (5b), and the output end of the second servo motor (5c) is connected with the threaded rod (5b 1).
9. The method for preparing a highly concentrated perfluorosulfonic acid solution according to claim 8, wherein the bottom of the top cover (5a) is provided with a partition (5a1), the inlet valve (6) and the outlet valve (7) are both provided on the top of the top cover (5a), and the inlet valve (6) and the outlet valve (7) are respectively provided on both sides of the partition (5a 1).
10. The method for preparing a high-concentration perfluorosulfonic acid solution according to claim 8, wherein the sealing mechanism (5) further comprises a door plate (5d) and a single-shaft cylinder (5e), the top cover (5a) is provided with a feeding port, the door plate (5d) is arranged at the feeding port, one side of the door plate (5d) is hinged with the top cover (5a), the fixed end of the single-shaft cylinder (5e) is hinged with the top of the top cover (5a), and the output end of the single-shaft cylinder (5e) is hinged with the door plate (5 d).
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Application publication date: 20211231 |