CN210287545U - Electrolysis device for synthesizing quaternary ammonium hydroxide - Google Patents
Electrolysis device for synthesizing quaternary ammonium hydroxide Download PDFInfo
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- CN210287545U CN210287545U CN201920779550.6U CN201920779550U CN210287545U CN 210287545 U CN210287545 U CN 210287545U CN 201920779550 U CN201920779550 U CN 201920779550U CN 210287545 U CN210287545 U CN 210287545U
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Abstract
The utility model relates to an electrolyzer for synthesizing quaternary ammonium hydroxide, the electrolyzer is a three-chamber two-diaphragm-plate-frame multipole type electrolyzer, a cation exchange membrane is arranged between a cathode chamber and an intermediate chamber in the three-chamber two-diaphragm-plate-frame multipole type electrolyzer, an anion exchange membrane is arranged between an anode chamber and the intermediate chamber, and the cation exchange membrane and the anion exchange membrane are respectively connected with a direct current voltage stabilizer through an electrode anode and an electrode cathode; the anolyte storage tank, the first infusion pump and the anode chamber are sequentially connected through an infusion pipe to form an anolyte loop; the raw material liquid storage tank, the second infusion pump and the middle chamber are sequentially connected through an infusion tube to form a raw material liquid loop. The cathode liquid storage tank, the third infusion pump and the cathode chamber are sequentially connected through an infusion tube to form an anolyte loop. The utility model discloses realize the control to multiple quaternary ammonium base production quality with PLC screen display control module, operating condition is stable in the production process, can carry out industrialization continuous production, and the electrolysis is efficient, and the electrolysis raffinate discharges lowly.
Description
Technical Field
The utility model relates to an electrolytic device for electrolytic synthesis quaternary ammonium base, in particular to an electrolytic device capable of continuously and industrially producing quaternary ammonium base.
Background
Quaternary ammonium hydroxide is an organic intermediate widely used in the fields of electronic chemicals (circuit board etchant and developer), organic synthesis, templating agents, phase transfer catalysts, and the like.
The common preparation methods of quaternary ammonium hydroxide are silver oxide method, potassium hydroxide method, alcohol metal method, ion exchange resin method, ion exchange membrane method, ion membrane electrodialysis method, etc. However, these methods do not produce highly pure quaternary ammonium hydroxide products, and the large amount of halide ions carried with them can be problematic for downstream applications.
In view of the above problems of the existing quaternary ammonium hydroxide preparation methods, it is desirable to provide an electrolysis apparatus for electrolyzing and synthesizing quaternary ammonium hydroxide, which can continuously electrolyze and prepare multi-quality quaternary ammonium hydroxide by using a three-chamber two-membrane electrolysis apparatus.
Disclosure of Invention
The utility model provides an electrolytic device of synthetic quaternary ammonium base to the singlechip realizes the control to multiple quaternary ammonium base production quality, and operating condition is stable in the production process, can carry out industrialization continuous production, and the electrolysis is efficient, and the electrolysis raffinate is discharged lowly.
The technical scheme of the utility model as follows:
an electrolyzer for synthesizing quaternary ammonium hydroxide comprises an anolyte storage tank, a raw material liquid storage tank, a catholyte storage tank, an electrolyzer and a PLC screen display control module, wherein the electrolyzer is a three-chamber two-diaphragm-plate-frame multipole type electrolyzer, a cation exchange membrane is arranged between a cathode chamber and an intermediate chamber in the three-chamber two-diaphragm-plate-frame multipole type electrolyzer, an anion exchange membrane is arranged between the anode chamber and the intermediate chamber, and the cation exchange membrane and the anion exchange membrane are respectively connected with a direct current voltage stabilizer through an electrode anode and an electrode cathode; the anolyte storage tank, the first infusion pump and the anode chamber are sequentially connected through an infusion pipe to form an anolyte loop; the raw material liquid storage tank, the second infusion pump and the middle chamber are sequentially connected through an infusion tube to form a raw material liquid loop; the cathode liquid storage tank, the third infusion pump and the cathode chamber are sequentially connected through an infusion tube to form an anolyte loop.
Further, the plate frame in the three-chamber two-membrane plate frame multi-electrode type electrolytic cell is made of one of polyethylene, polypropylene, acrylic plates, polytetrafluoroethylene and ABS resin.
Further, the electrode anode and the electrode cathode are made of one of a titanium material, a nickel material and a stainless steel electrode plated with ruthenium iridium and iridium tantalum.
Furthermore, the anode and the cathode of the electrode are reticular titanium-based noble metal coating electrodes, and the coating is RuO2-TiO2Or IrO2-Ta2O5。
Further, the cation exchange membrane is one of fluorine-containing polyethylene, polypropylene, polystyrene and polyacrylic acid containing sulfonic acid functional groups.
Further, the anion exchange membrane is one of fluorine-containing polyethylene, polypropylene, polystyrene and polyacrylic acid containing carboxylic acid or quaternary ammonium functional groups.
Further, the cation exchange membrane is a perfluoropolymer cation exchange membrane; the anion exchange membrane is a perfluorinated polymer anion exchange membrane.
Furthermore, heat exchangers are respectively arranged in the anolyte storage tank, the raw material liquid storage tank and the catholyte storage tank, are tubular heat exchangers and are used for adjusting the temperature of the electrolyte, and are respectively provided with a water level monitor and a temperature sensor.
Further, a pH meter is arranged in the anode liquid storage tank and used for testing the pH value of the anode liquid; the first transfer pump is equipped with first flow controller on the inlet tube that is connected with the anode chamber, and the second transfer pump is equipped with the second flow controller on the inlet tube that is connected with the intermediate chamber, and the third transfer pump is equipped with the third flow controller on the inlet tube that is connected with the cathode chamber.
Furthermore, the PLC screen display control module is respectively connected with the first flow controller, the second flow controller, the third flow controller, the direct current voltage stabilizer, the first infusion pump, the second infusion pump, the third infusion pump, the pH meter and the direct current voltage stabilizer, signal acquisition and processing are carried out by the PLC screen display control module, and the PLC screen display control module is connected with the screen for interactive operation and used for checking and regulating the working state of each working component from time to time.
The utility model has the advantages that:
the utility model overcomes the defect that only single variety of quaternary ammonium hydroxide products can be prepared in the traditional preparation method, can prepare various quaternary ammonium hydroxide products such as tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide, tetrapropyl ammonium hydroxide and the like, and the products can directly obtain the solution sold in the market with the concentration of 20 percent, thereby effectively reducing the preparation cost and improving the economic benefit; on the other hand, compared with the existing single-membrane electrolysis device, the three-chamber two-membrane electrolysis device is adopted, so that the device can be prevented from being damaged and polluting the environment due to halogen formation, and the device is pollution-free green synthesis electrolysis equipment. In addition, the device carries a singlechip and a touch screen interface, and can be adjusted at any time to monitor the whole electrolysis process.
Drawings
FIG. 1 is a system diagram of an electrolyzer for synthesizing quaternary ammonium hydroxide according to the present invention.
Detailed Description
The structure, shape and features of the present invention will be described in further detail with reference to the embodiments and the accompanying drawings. It should be understood that the following examples are illustrative of the present invention, but are not intended to limit the scope of the present invention.
As shown in figure 1, the electrolyzer for synthesizing quaternary ammonium hydroxide comprises a direct current voltage stabilizer 13, a liquid conveying pipe 4, an anode liquid storage tank 1, a raw material liquid storage tank 2, a cathode liquid storage tank 3, a tubular heat exchanger 15, a valve 16, a first liquid conveying pump 19, a second liquid conveying pump 18, a third liquid conveying pump 17, a first flow controller 20, a second flow controller 21, a third flow controller 22, an electrolytic bath 5 and a PLC screen display control module 14.
The electrolytic cell 5 is a three-chamber two-membrane plate frame multipole type electrolytic cell, and comprises a cathode chamber 6, an intermediate chamber 9, an anode chamber 12, an anion exchange membrane 10, a cation exchange membrane 8, an electrode anode 11 and an electrode cathode 7. The cathode chamber 6 is connected with the anode chamber 12 through the middle chamber 9, the cation exchange membrane 8 is arranged between the cathode chamber 6 and the middle chamber 9, the anion exchange membrane 10 is arranged between the anode chamber 12 and the middle chamber 9, and the anion exchange membrane 10 and the cation exchange membrane 8 are respectively connected with the direct current voltage stabilizer 13 through the electrode anode 11 and the electrode cathode 7.
The anolyte storage tank 1, the first infusion pump 19 and the anode chamber 12 are connected in sequence through infusion tubes to form an anolyte loop. The raw material liquid storage tank 2, the second infusion pump 18 and the intermediate chamber 9 are connected in sequence through an infusion tube to form a raw material liquid loop. The cathode liquid storage tank 3, the third infusion pump 17 and the cathode chamber 6 are connected in sequence through infusion tubes to form an anolyte loop.
A first flow controller 20 is arranged on a water inlet pipe of the first infusion pump 19 connected with the anode chamber 12, a second flow controller 21 is arranged on a water inlet pipe of the second infusion pump 18 connected with the intermediate chamber 9, and a third flow controller 22 is arranged on a water inlet pipe of the third infusion pump 17 connected with the cathode chamber 6.
The plate frame in the three-chamber two-plate frame multi-pole electrolytic cell is made of one of polyethylene, polypropylene, acrylic plates, polytetrafluoroethylene and ABS resin, and is preferably made of polytetrafluoroethylene.
The electrode anode 11 and the electrode cathode 7 are one of a titanium material, a nickel material and a stainless steel electrode plated with ruthenium iridium and iridium tantalum. Preferably a reticular titanium-based noble metal coating electrode, and the coating is RuO2-TiO2Or IrO2-Ta2O5The coating is preferably RuO2-TiO2。
The cation exchange membrane 10 is one of fluorine-containing polyethylene, polypropylene, polystyrene and polyacrylic acid containing sulfonic acid functional groups. Preferably a perfluoropolymer cation exchange membrane. The anion exchange membrane 8 is one of fluorine-containing polyethylene, polypropylene, polystyrene and polyacrylic acid containing carboxylic acid or quaternary ammonium functional groups. Preferably a perfluoropolymer anion exchange membrane.
The first flow controller 20, the second flow controller 21, the third flow controller 22, the direct current voltage stabilizer 13, the first infusion pump 19, the second infusion pump 18, the third infusion pump 17, the pH meter and the direct current stabilized voltage power supply are respectively connected with the PLC screen display control module 14. The PLC screen display control module 14 is used for signal acquisition and processing, and the interactive operation screen connection is used for checking and regulating the working state of each working component from time to time.
Application example 1:
adding 5% ammonium chloride solution into an anode storage tank, adjusting the pH value to be about 3 by hydrochloric acid, adding 45% tetraethylammonium hydrobromide solution into a raw material solution storage tank, adding 5% tetraethylammonium hydrobromide solution into a cathode solution storage tank, and starting a magnetic pump to circulate each chamber.
The power supply of the direct current voltage stabilizer is switched on, the constant current electrolysis is carried out by adopting the method of continuous electrolysis of constant voltage current and the current of 200A, and the voltage of the electrolytic tank is stabilized at 6.5-7.2V after the electrolysis.
The degree of the liquid storage tanks is controlled to be 40 ℃ through a control panel, the inflow rate of water is controlled to be 5L/min by a monitoring flowmeter, and the acidity of the anolyte is controlled by a pH meter for monitoring the anolyte.
After 24 hours of continuous electrolysis, tetraethyl ammonium hydroxide solution with the product quality of 22 percent is obtained, the bromide ion concentration is 110ppm, and the current efficiency is 58 percent.
Application example 2:
according to the electrolysis device of the embodiment 1, the raw material solution is replaced by tetrapropylammonium bromide, and after 24 hours of continuous electrolysis, a tetrapropylammonium hydroxide solution with the product quality of 20 percent is obtained, the bromide ion concentration of 140ppm and the current efficiency of 52 percent.
Application example 3:
according to the electrolysis device of the embodiment 1, the raw material solution is replaced by tetramethylammonium chloride, and after 24 hours of continuous electrolysis, tetrapropylammonium hydroxide solution with the product quality of 25 percent is obtained, the bromide ion concentration is 70ppm, and the current efficiency is 68 percent.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. The utility model provides an electrolytic device of synthetic quaternary ammonium hydroxide, includes anolyte storage tank, raw materials liquid storage tank, catholyte storage tank, electrolysis trough, PLC screen display control module, its characterized in that: the electrolytic cell is a three-chamber two-diaphragm-plate-frame multi-pole electrolytic cell, a cation exchange membrane is arranged between a cathode chamber and an intermediate chamber in the three-chamber two-diaphragm-plate-frame multi-pole electrolytic cell, an anion exchange membrane is arranged between an anode chamber and the intermediate chamber, and the cation exchange membrane and the anion exchange membrane are respectively connected with a direct current voltage stabilizer through an electrode anode and an electrode cathode; the anolyte storage tank, the first infusion pump and the anode chamber are sequentially connected through an infusion pipe to form an anolyte loop; the raw material liquid storage tank, the second infusion pump and the middle chamber are sequentially connected through an infusion tube to form a raw material liquid loop; the cathode liquid storage tank, the third infusion pump and the cathode chamber are sequentially connected through an infusion tube to form an anolyte loop.
2. An electrolysis apparatus for the synthesis of quaternary ammonium hydroxide according to claim 1, wherein: the plate frame in the three-chamber two-membrane plate frame multipole type electrolytic cell is made of one of polyethylene, polypropylene, acrylic plates, polytetrafluoroethylene and ABS resin.
3. An electrolysis apparatus for the synthesis of quaternary ammonium hydroxide according to claim 1, wherein: the electrode anode and the electrode cathode are made of one of a titanium material, a nickel material and a stainless steel electrode which are plated with ruthenium iridium and iridium tantalum.
4.An electrolysis apparatus for the synthesis of quaternary ammonium hydroxide according to claim 1, wherein: the anode and the cathode of the electrode are mesh titanium-based noble metal coating electrodes, and the coating is RuO2-TiO2Or IrO2-Ta2O5。
5. An electrolysis apparatus for the synthesis of quaternary ammonium hydroxide according to claim 1, wherein: the cation exchange membrane is one of fluorine-containing polyethylene, polypropylene, polystyrene and polyacrylic acid containing sulfonic acid functional groups.
6. An electrolysis apparatus for the synthesis of quaternary ammonium hydroxide according to claim 1, wherein: the anion exchange membrane is one of fluorine-containing polyethylene, polypropylene, polystyrene and polyacrylic acid containing carboxylic acid or quaternary ammonium functional groups.
7. An electrolysis apparatus for the synthesis of quaternary ammonium hydroxide according to claim 1, wherein: the cation exchange membrane is a perfluorinated polymer cation exchange membrane, and the anion exchange membrane is a perfluorinated polymer anion exchange membrane.
8. An electrolysis apparatus for the synthesis of quaternary ammonium hydroxide according to claim 1, wherein: and heat exchangers are respectively arranged in the anolyte storage tank, the raw material liquid storage tank and the catholyte storage tank, are tubular heat exchangers and are used for adjusting the temperature of the electrolyte, and are respectively provided with a water level monitor and a temperature sensor.
9. An electrolysis apparatus for the synthesis of quaternary ammonium hydroxide according to claim 1, wherein: a pH meter is arranged in the anode liquid storage tank and used for testing the pH value of the anode liquid; the first transfer pump is equipped with first flow controller on the inlet tube that is connected with the anode chamber, and the second transfer pump is equipped with the second flow controller on the inlet tube that is connected with the intermediate chamber, and the third transfer pump is equipped with the third flow controller on the inlet tube that is connected with the cathode chamber.
10. An electrolysis apparatus for the synthesis of quaternary ammonium hydroxide according to claim 1, wherein: the PLC screen display control module is respectively connected with the first flow controller, the second flow controller, the third flow controller, the direct current voltage stabilizer, the first infusion pump, the second infusion pump, the third infusion pump, the pH meter and the direct current voltage stabilizing power supply, signal acquisition and processing are carried out by the PLC screen display control module, and the PLC screen display control module is connected with the screen in an interactive operation mode and used for checking and regulating the working state of each working component at any time.
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