CN220057049U - Tetraethylammonium hydroxide synthesizer - Google Patents
Tetraethylammonium hydroxide synthesizer Download PDFInfo
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- CN220057049U CN220057049U CN202321105845.8U CN202321105845U CN220057049U CN 220057049 U CN220057049 U CN 220057049U CN 202321105845 U CN202321105845 U CN 202321105845U CN 220057049 U CN220057049 U CN 220057049U
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- 229940073455 tetraethylammonium hydroxide Drugs 0.000 title claims abstract description 45
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 title claims abstract description 45
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 239000003513 alkali Substances 0.000 claims abstract description 17
- 239000012528 membrane Substances 0.000 claims abstract description 16
- 238000000576 coating method Methods 0.000 claims description 35
- 239000011248 coating agent Substances 0.000 claims description 33
- 238000012546 transfer Methods 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000005868 electrolysis reaction Methods 0.000 claims description 16
- 238000003786 synthesis reaction Methods 0.000 claims description 14
- 230000015572 biosynthetic process Effects 0.000 claims description 13
- 239000003011 anion exchange membrane Substances 0.000 claims description 9
- 238000005341 cation exchange Methods 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 9
- 230000008020 evaporation Effects 0.000 claims description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 8
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims description 8
- 239000004020 conductor Substances 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 6
- 239000002344 surface layer Substances 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 229910052741 iridium Inorganic materials 0.000 claims description 4
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910001925 ruthenium oxide Inorganic materials 0.000 claims description 3
- -1 hydroxide ions Chemical class 0.000 abstract description 24
- 239000000460 chlorine Substances 0.000 abstract description 16
- 229910052801 chlorine Inorganic materials 0.000 abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 13
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 11
- 239000001301 oxygen Substances 0.000 abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 abstract description 11
- 239000003792 electrolyte Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 10
- YMBCJWGVCUEGHA-UHFFFAOYSA-M tetraethylammonium chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC YMBCJWGVCUEGHA-UHFFFAOYSA-M 0.000 abstract description 9
- 150000002500 ions Chemical class 0.000 abstract description 7
- 239000007788 liquid Substances 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000001257 hydrogen Substances 0.000 description 12
- 229910052739 hydrogen Inorganic materials 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 229960003750 ethyl chloride Drugs 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 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
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000003444 phase transfer catalyst Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The utility model provides a tetraethylammonium hydroxide synthesizer, which divides chloride ions in raw material tetraethylammonium chloride by arranging an anode region, a raw material region and a cathode region, reduces the concentration of the chloride ions in the anode region, and simultaneously, an alkali metering pump is arranged in the anode region to adjust the electrolyte in the anode region to be alkaline and increase OH ‑ The concentration of the electrolyte ensures that chloride ions are not discharged at the anode, hydroxide ions are discharged, so that the anode generates oxygen, and through the combination of the means, the generation of chlorine in the anode region in the process of producing tetraethylammonium hydroxide can be avoided, and the problems that the anode is easy to generate chlorine and damage is caused to the electrolytic tank and an ion membrane when the tetraethylammonium hydroxide is synthesized in an electrolytic mode by adopting a two-chamber electrolytic tank consisting of a cathode tank and an anode tank are solved.
Description
Technical Field
The utility model relates to the technical field of quaternary ammonium hydroxide synthesis, in particular to a tetraethylammonium hydroxide synthesis device.
Background
Tetraethylammonium hydroxide (TEAH) is a common chemical product on the market and is widely used, mainly as a template agent, a phase transfer catalyst, a petroleum industry impurity removing agent, and the like. Tetraethylammonium hydroxide is an essential intermediate for promoting the development of organic synthesis, medicine, petroleum and other industries. The synthesis of tetraethylammonium chloride, an intermediate for tetraethylammonium hydroxide, is generally carried out by reacting triethylamine and ethyl chloride in an organic solvent. As for the preparation of tetraethylammonium hydroxide by the intermediate tetraethylammonium chloride, a silver oxide method, an alkali displacement method, an ion exchange resin method are generally used. These methods have the common problems of high production cost, poor product quality, difficulty in mass production and the like. And wastewater containing quaternary ammonium compounds, which is difficult to treat, is generated in the preparation process, so that adverse environmental effects are caused. Under the large environment with higher and higher requirements on environmental protection, the traditional tetraethylammonium hydroxide production method is difficult to meet the requirements.
Thus, a method for preparing tetraethylammonium hydroxide by electrolysis has been developed, namely, raw tetraethylammonium chloride is electrolyzed by a two-chamber electrolytic tank consisting of a cathode tank and an anode tank, and the product tetraethylammonium hydroxide is obtained in the cathode tank, and the following reaction occurs:
reaction at anode:
(CH 3 CH 2 ) 4 NCl→(CH 3 CH 2 ) 4 N + +Cl-
2Cl-→Cl 2
reaction at cathode
(CH 3 CH 2 ) 4 N + +OH-→(CH 3 CH 2 ) 4 NOH
2H + →H 2
As is evident from the above reaction, this electrolysis method is prone to precipitate toxic and harmful chlorine gas at the anode, and although the chlorine gas can be recovered, the oxidizing property of the chlorine gas itself and hypochlorite generated by the reaction with water inevitably damages the electrolytic cell and the ion membrane, and the dry film is generated due to the generation of gas, thereby damaging the ion membrane.
Disclosure of Invention
The utility model provides a tetraethylammonium hydroxide synthesizer which is used for solving the problem that the electrolytic tank and an ion membrane are damaged by chlorine easily generated by an anode when the tetraethylammonium hydroxide is synthesized in an electrolytic way by adopting the two-chamber electrolytic tank consisting of a cathode tank and an anode tank.
The utility model provides a tetraethylammonium hydroxide synthesizer, which comprises an electrolytic reaction tank, wherein the electrolytic reaction tank is divided into an anode area, a raw material area and a cathode area by an anion exchange membrane and a cation exchange membrane;
an acidometer and an electrolysis anode are arranged in the anode region, and the electrolysis anode is close to the anion exchange membrane; the anode region is connected with an alkali metering pump; the anode region is also connected with a first transfer pump and a first heat exchanger in series in turn to form a loop;
an alkalinity meter is arranged at the upper part in the cathode region, and an electrolytic cathode is arranged at a position close to the cation exchange membrane; the cathode region is sequentially connected with the vacuum pump and the air storage tank; the cathode region is also connected with a second transfer pump and a second heat exchanger in series in turn to form a loop.
Optionally, a first heating coil and a second heating coil are arranged in the raw material area, and the input end of the first heating coil is connected with the output end of a heat exchange medium of the first heat exchanger;
the input end of the second heating coil is connected with the heat exchange medium output end of the second heat exchanger.
Optionally, the second transfer pump and the second heat exchanger are connected with the evaporation concentrator through a three-way valve.
Optionally, the acidometer and the alkali metering pump are electrically connected with the controller.
Optionally, the electrolytic anode is a net structure made of inert conductive substances with anode coatings fixed on the surface layers; the inert conductive material is titanium, platinum, palladium and other metals or graphite; the anode coating is made of tin coating, iridium coating or ruthenium oxide coating.
Optionally, the electrolytic cathode is a net-shaped structure made of conductive materials with cathode coatings fixed on the surface layers;
the cathode coating is a nickel-aluminum porous coating or a cobaltosic oxide coating.
Alternatively, the evaporative concentrator is a 3-4 effect MVR evaporator.
According to the device, chloride ions in tetraethylammonium chloride serving as a raw material are split by arranging the anode area, the raw material area and the cathode area, so that the concentration of the chloride ions in the anode area is reduced, meanwhile, an alkali metering pump is arranged in the anode area, the electrolyte in the anode area is regulated to be alkaline, and the concentration of OH < - > is increased, so that the situation that the chloride ions are not discharged at the anode and the hydroxide ions are discharged is ensured, so that the anode generates oxygen, the generation of chlorine in the anode area in the process of producing tetraethylammonium hydroxide can be avoided by combining the means, and the problem that the anode is easy to generate chlorine when the tetraethylammonium hydroxide is synthesized in an electrolysis mode in the existing two-chamber electrolytic tank consisting of a cathode tank and an anode tank is solved, and the problem that the electrolytic tank and an ion membrane are damaged is solved.
Drawings
In order to more clearly illustrate the embodiments of the present utility model or the technical solutions of the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are some embodiments of the present utility model, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic diagram of a tetraethylammonium hydroxide synthesizing apparatus according to an embodiment of the utility model;
fig. 2 is a schematic diagram of a tetraethylammonium hydroxide synthesis apparatus according to another embodiment of the utility model;
fig. 3 is a schematic diagram of a tetraethylammonium hydroxide synthesis apparatus according to another embodiment of the utility model;
fig. 4 is a schematic diagram of a tetraethylammonium hydroxide synthesis apparatus according to another embodiment of the utility model.
Reference numerals illustrate:
1. an electrolytic reaction tank; 2. an alkali metering pump; 3. a first transfer pump; 4. a first heat exchanger; 5. a vacuum pump; 6. a second transfer pump; 7. a second heat exchanger; 8. an evaporative concentrator; 9. a controller; 10. a raw material zone; 11. an anode region; 12. a cathode region; 51. a gas storage tank; 81. a three-way valve; 100. an anion exchange membrane; 101. a first heating coil; 102. a second heating coil; 200. a cation exchange membrane; 1101. an acidometer; 1102. an electrolytic anode; 1201. an alkalinity meter; 1202. and (3) electrolyzing the cathode.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present utility model more clear, the technical solutions in the embodiments of the present utility model will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are also within the scope of the utility model.
As shown in fig. 1, the present utility model provides a tetraethylammonium hydroxide synthesizing device, comprising an electrolytic reaction tank 1, wherein the electrolytic reaction tank 1 is divided into an anode region 11, a raw material region 10 and a cathode region 12 by an anion exchange membrane 100 and a cation exchange membrane 200;
an acidometer 1101 and an electrolysis anode 1102 are arranged in the anode region 11, and the electrolysis anode 1102 is close to the anion exchange membrane 100; the anode region 11 is connected with an alkali metering pump 2; the anode region 11 is also connected with the first transfer pump 3 and the first heat exchanger 4 in series in turn to form a loop;
an alkalinity meter 1201 and an electrolysis cathode 1202 are arranged in the cathode region 12, and the electrolysis cathode 1202 is close to the cation exchange membrane 200; the cathode region 12 is connected with the vacuum pump 5 and the air storage tank 51 in sequence; the cathode region 12 is also connected with the second transfer pump 6 and the second heat exchanger 7 in series in turn to form a loop.
In the device of the utility model, the anode region 11 is connected with the alkali metering pump 2, the electrolyte of the anode region 11 is made alkaline, under the condition, tetraethylammonium chloride is adopted for electrolysis to produce tetraethylammonium hydroxide, and the reaction process is as follows:
raw material area:
(CH 3 CH 2 ) 4 NCl→(CH 3 CH 2 ) 4 N + +Cl-
reaction at anode:
H + +Cl-→HCl
2H 2 O-4e→4H + +O 2
reaction at the cathode:
(CH 3 CH 2 ) 4 N + +OH-→(CH 3 CH 2 ) 4 NOH
2H + →H 2 ；
because in the scheme of the utility model, the anode region 11 is adjusted to be in an alkaline state, the concentration of OH < - > is increased, and the chlorine ions are ensured not to discharge at the anode, so that the electrode reaction of hydroxyl ion discharge releasing oxygen occurs in the anode region 11, and the generation of chlorine is avoided.
In the utility model, the first transfer pump 3 and the first heat exchanger 4 are arranged, so that the heat exchange of the anolyte can be realized while the anolyte is circulated, and the anolyte is circulated by adopting the transfer pump, and the anolyte can be stirred without an additional stirring device. Similarly, the second transfer pump 6 and the second heat exchanger 7 function as the first transfer pump 3 and the first heat exchanger 4 described above, and will not be described again here.
In the utility model, the vacuum pump 5 pumps the cathode region 12 to be in a micro negative pressure state, so that the hydrogen generated by the cathode region 12 can be discharged in time, adverse effects caused by hydrogen accumulation are avoided, and meanwhile, the circulation of the cathode liquid by the second transfer pump 6 is not influenced.
An electrolytic raw material tetraethylammonium chloride aqueous solution (concentration: 1 to 4 mol/L) is added to the raw material zone 10, clean water is added to the anode zone 11 and sodium hydroxide is added to adjust the pH to 11 to 13, distilled water is added to the cathode zone 12, and a small amount of tetraethylammonium hydroxide (conductivity is increased) is added so that the initial concentration thereof is 0.8 to 1.2mol/L. Simultaneously starting the first transfer pump 3 and the second heat exchanger 7, after the heat exchange of the raw material area 10, the cathode area 12 and the anode area 11 is stable (the temperature of the detection liquid is 70-85 ℃, the temperature of the liquid in the raw material area 10 is 70-75 ℃), connecting the electrolytic anode 1102 with the positive electrode of a direct current power supply, connecting the electrolytic cathode 1202 with the negative electrode of the direct current power supply, and controlling the current density to be 1000-1200A/m 2; simultaneously, the vacuum pump 5 is started to vacuumize the cathode region 12, so that the cathode region 12 is kept in a micro negative pressure state (-0.002-0.006 MPa).
In the reaction, chloride ions penetrate through the anion exchange membrane 100 and enter the anode region 11, and as the electrolyte in the anode region 11 is alkaline, chlorine ions are ensured not to be discharged at the anode and cannot be generated, at the moment, hydroxide ions are discharged at the anode, so that oxygen is generated in the anode region 11, and the generation of chlorine is avoided; while tetraethylammonium cations enter the cathode region 12 through the cation exchange membrane 200, hydrogen ions in water molecules in the cathode region 12 are electronically generated to generate hydrogen, and in the hydroxide ion electrolyte, the hydrogen ions are combined with the tetraethylammonium cations to generate tetraethylammonium hydroxide, namely a product.
During the reaction, the acidimeter 1101 detects that the pH of the anode region 11 falls below a preset low value (such as 8), and an operator can add an alkali solution (such as 10-20 wt% sodium hydroxide aqueous solution) to the anode region 11 through the alkali metering pump 2 to neutralize hydrogen ions generated in the anode region, and adjust the pH in the anode region 11 to increase OH - Thereby ensuring that chlorine ions are not discharged at the anode and hydroxide ions are discharged, so that the anode generates oxygen, and the generation of chlorine gas is avoided to cause the environment and the ion membraneDamage, the oxygen produced can be discharged directly; in the cathode region, hydrogen gas is generated, which is a flammable and explosive gas, so that the hydrogen gas generated in the cathode region 12 is sucked and stored in the gas storage tank 51 by the vacuum pump 5 to be intensively processed. When the alkalinity meter 1201 detects that the high value of hydroxide ions therein reaches a certain concentration, the aqueous solution of tetraethylammonium hydroxide in the cathode region 12 may be diverted to be concentrated, crystallized, and distilled water may be simultaneously fed into the cathode region 12.
Similarly, when the liquid in the anode region 11 runs for a certain time, the liquid should be sampled and analyzed, and if the concentration of the salt is too high, the liquid should be turned out to be neutralized and concentrated to recover the salt and simultaneously the alkaline liquid should be supplemented.
The device of the utility model divides the chloride ions in the raw material tetraethylammonium chloride by arranging the anode region 11, the raw material region 10 and the cathode region 12, reduces the concentration of the chloride ions in the anode region 11, and simultaneously, the anode region 11 is provided with the alkali metering pump 2, adjusts the electrolyte in the anode region to be alkaline and increases OH - The concentration of the electrolyte ensures that chloride ions are not discharged at the anode, hydroxide ions are discharged, so that the anode generates oxygen, and through the combination of the two means, the generation of chlorine in the anode region 11 in the process of producing tetraethylammonium hydroxide can be avoided, and the problems that the anode is easy to generate chlorine and damage is caused to the electrolytic tank and an ion membrane when the tetraethylammonium hydroxide is synthesized in an electrolytic mode by adopting a two-chamber electrolytic tank consisting of a cathode tank and an anode tank are solved. In addition, the vacuum pump 2 is arranged to timely discharge the hydrogen generated in the cathode region 12, so that negative effects such as dry films and the like caused by accumulation of the hydrogen in the cathode region 12 are avoided.
Optionally, as shown in fig. 2, a first heating coil 101 and a second heating coil 102 are disposed in the raw material area 10, and an input end of the first heating coil 101 is connected with an output end of a heat exchange medium of the first heat exchanger 4;
the input end of the second heating coil 102 is connected with the heat exchange medium output end of the second heat exchanger 7.
In the utility model, the first heating coil 101 and the second heating coil 102 are arranged to preheat the liquid in the raw material zone 10, and the heat exchange media in the first heating coil 101 and the second heating coil 102 come from the first heat exchanger 4 and the second heat exchanger 7 respectively, so that the heat exchange media in the heat exchangers can be utilized in a gradient manner, the energy loss is reduced, and the production cost of enterprises is reduced.
Alternatively, as shown in fig. 3, the second transfer pump 6 and the second heat exchanger 7 are connected to the evaporation concentrator 8 through a three-way valve 81.
In the utility model, the evaporation concentrator 8 is arranged to concentrate tetraethylammonium hydroxide with preset concentration in the cathode region 12, and the three-way valve 81 is convenient for switching the communication state of the second transfer pump 6, the second heat exchanger 7 and the three-way valve 81.
Alternatively, as shown in fig. 4, both the acidometer 1101 and the alkali metering pump 2 are electrically connected to the controller 9.
In the utility model, the acidometer 1101 and the alkali metering pump 2 are both electrically connected with the controller 9, and the controller 9 can be utilized to realize real-time and automatic control of the pH value in the anode region 11. In an alternative implementation, level gauges are provided in the cathode region 12 and the anode region 11, and are connected to the controller 9, an alkalinity gauge 1201 and a three-way valve 81 are also connected to the controller 9,
optionally, the electrolytic anode 1102 is a net structure made of inert conductive material with an anode coating fixed on the surface layer; the inert conductive material is titanium, platinum, palladium and other metals or graphite; the anode coating is made of tin coating, iridium coating or ruthenium oxide coating.
In the present utility model, the electrolytic anode 1102 discharges to lose electrons in the electrolytic reaction, and oxidation reaction occurs, so that an inert substance is required to serve as an anode electrode. Graphite has the advantages of low cost and availability, and the material selected as the anode electrode, and inert metals such as titanium, platinum, palladium and the like have the advantages of difficult corrosion and long service life. The anode coating is coated on the anode electrode, so that the reaction efficiency of the anode can be enhanced; the anode electrode is made into a net shape, so that a larger specific surface area can be provided, and the electrolysis efficiency is improved. The ruthenium dioxide coating can work under high current density, has lower cell voltage and good chemical stability, so that the ruthenium dioxide coating can save electricity, reduce cost and save energy. The tin coating and the iridium coating are added into the anode coating, so that the overpotential of oxygen can be increased, and the selectivity of the anode can be improved.
Optionally, the electrolytic cathode 1202 is a mesh structure made of a conductive material with a cathode coating fixed on the surface layer;
the cathode coating is a nickel-aluminum porous coating or a cobaltosic oxide coating.
In the present utility model, in the electrolysis process, the electrolytic cathode 1202 obtains electrons in the electrolysis reaction, and a reduction reaction occurs, so that a conductive substance such as nickel, low carbon steel, or the like can be selected as a cathode electrode. The electrolytic cathode 1202 is net-shaped, and can provide larger specific surface area, thereby improving electrolytic efficiency, and nickel-aluminum porous coating or cobaltosic oxide coating can be added to reduce voltage loss during electrolysis and save cost.
Alternatively, the evaporative concentrator 8 is a 3-4 effect MVR evaporator.
In the utility model, the evaporation concentrator 8 selects a 3-effect or 4-effect MVR evaporator, so that the usage amount of steam can be reduced, the energy utilization efficiency is improved, and the production cost is saved.
A tetraethylammonium hydroxide synthesizer, its working process is as follows:
an electrolytic raw material tetraethylammonium chloride aqueous solution (concentration: 1 to 4 mol/L) is added to the raw material zone 10, clean water is added to the anode zone 11 and sodium hydroxide is added to adjust the pH to 11 to 13, distilled water is added to the cathode zone 12, and a small amount of tetraethylammonium hydroxide (conductivity is increased) is added so that the initial concentration thereof is 0.8 to 1.2mol/L. The three-way valve 81 is adjusted to a state of communicating the second transfer pump 6 with the second heat exchanger 7 to block the evaporation concentrator 8. Simultaneously starting the first transfer pump 3 and the second heat exchanger 7, after the heat exchange of the raw material zone 10, the cathode zone 12 and the anode zone 11 is stable (the temperature of detection liquid is 70-85 ℃ and the temperature of liquid in the raw material zone 10 is 70-75 ℃), connecting the electrolytic anode 1102 with the positive electrode of a direct current power supply, connecting the electrolytic cathode 1202 with the negative electrode of the direct current power supply, and controlling the current density to be 1000-1200A/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Simultaneously, the vacuum pump 5 is started to vacuumize the cathode region 12, so that the cathode region 12 is kept in a micro negative pressure state.
In the reaction, chloride ions permeate through the anion exchange membrane 100 to enter the anode region 11, and the electrolyte in the anode region 11 is alkaline, so that the concentration of chloride ions is increasedLarge OH - Thereby ensuring that chloride ions are not discharged at the anode and hydroxide ions are discharged, so that the anode region 11 generates oxygen, and the generation of chlorine is avoided; while tetraethylammonium cations enter the cathode region 12 through the cation exchange membrane 200, hydrogen ions in water molecules in the cathode region 12 are electronically generated to generate hydrogen, and in the hydroxide ion electrolyte, the hydrogen ions are combined with the tetraethylammonium cations to generate tetraethylammonium hydroxide, namely a product.
The acidimeter 1101 detects that the pH of the anode region 11 falls below a preset low value (such as 8) in the reaction process, and feeds data back to the controller 9, the controller 9 controls the alkali metering pump 2 to add alkali liquor (such as 10-20%wt sodium hydroxide aqueous solution) into the anode region 11, timely neutralize hydrogen ions generated in the anode region, adjust the pH in the anode region 11 and increase OH - Thereby ensuring that chlorine ions are not discharged at the anode and hydroxide ions are discharged, so that the anode generates oxygen, the damage to the environment and the ionic membrane caused by the generation of chlorine is avoided, and the generated oxygen can be directly discharged; in the cathode region, hydrogen gas is generated, which is a flammable and explosive gas, so that the hydrogen gas generated in the cathode region 12 is sucked and stored in the gas storage tank 51 by the vacuum pump 5 to be intensively processed. When the alkalinity meter 1201 detects that the high value of hydroxide ions therein reaches a certain concentration, the three-way valve 81 is adjusted to be communicated with the second transfer pump 6 and the evaporation concentrator 8 to block the second heat exchanger 7, tetraethylammonium hydroxide therein is transferred into the evaporation concentrator 8 to be concentrated, distilled water is supplemented into the cathode region 12 at the same time, when the alkalinity meter 1201 detects that the low value of hydroxide ions therein reaches a certain concentration, the three-way valve 81 is adjusted to be communicated with the second transfer pump 6 and the second heat exchanger 7 to block the evaporation concentrator 8 to continue to produce tetraethylammonium hydroxide, in production, a liquid level meter can be arranged in the cathode region 12 and the anode region 11 and connected with the controller 9, the alkalinity meter 1201 and the three-way valve 81 are also connected with the controller 9, thereby realizing automatic control of the tetraethylammonium hydroxide production process, and simultaneously realizing continuous production of the tetraethylammonium hydroxide.
Similarly, when the liquid in the anode region 11 runs for a certain time, the liquid therein should be sampled and analyzed, and if the concentration of the salt therein increases, the liquid should be transferred out for neutralization and concentration treatment to recover the salt therein and simultaneously be supplemented with alkaline liquid.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solution of the present utility model, and not limiting thereof; although the utility model has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art will appreciate that; the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the utility model.
Claims (7)
1. The tetraethylammonium hydroxide synthesis device is characterized by comprising an electrolytic reaction tank (1), wherein the electrolytic reaction tank (1) is divided into an anode region (11), a raw material region (10) and a cathode region (12) by an anion exchange membrane (100) and a cation exchange membrane (200);
an acidometer (1101) and an electrolysis anode (1102) are arranged in the anode region (11), and the electrolysis anode (1102) is close to the anion exchange membrane (100); the anode region (11) is connected with an alkali metering pump (2); the anode region (11) is also sequentially connected with the first transfer pump (3) and the first heat exchanger (4) in series to form a loop;
an alkalinity meter (1201) is arranged in the cathode region (12), and an electrolytic cathode (1202) is arranged at a position close to the cation exchange membrane (200); the cathode region (12) is sequentially connected with the vacuum pump (5) and the air storage tank (51); the cathode region (12) is also connected with the second transfer pump (6) and the second heat exchanger (7) in series in turn to form a loop.
2. The tetraethylammonium hydroxide synthesis device according to claim 1, wherein a first heating coil (101) and a second heating coil (102) are arranged in the raw material zone (10), and an input end of the first heating coil (101) is connected with a heat exchange medium output end of the first heat exchanger (4);
the input end of the second heating coil (102) is connected with the heat exchange medium output end of the second heat exchanger (7).
3. The tetraethylammonium hydroxide synthesis device according to claim 1, wherein the second transfer pump (6) and the second heat exchanger (7) are connected to the evaporation concentrator (8) through a three-way valve (81).
4. The tetraethylammonium hydroxide synthesis device according to claim 1, wherein the acidometer (1101) and the alkali metering pump (2) are both electrically connected to a controller (9).
5. The tetraethylammonium hydroxide synthesis device according to claim 1, wherein the electrolytic anode (1102) is a mesh structure made of an inert conductive material with an anode coating fixed on a surface layer; the inert conductive material is metal or graphite; the anode coating is made of tin coating, iridium coating or ruthenium oxide coating; the metal is titanium, platinum or palladium.
6. The tetraethylammonium hydroxide synthesis device according to claim 1, wherein the electrolytic cathode (1202) is a mesh structure made of a conductive material with a cathode coating fixed to a surface layer;
the cathode coating is a nickel-aluminum porous coating or a cobaltosic oxide coating.
7. A tetraethylammonium hydroxide synthesis apparatus according to claim 3, wherein the evaporative concentrator (8) is a 3-4 effect MVR evaporator.
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