CN113981476A - Preparation method of energy-saving tetraethylammonium hydroxide with high production efficiency - Google Patents
Preparation method of energy-saving tetraethylammonium hydroxide with high production efficiency Download PDFInfo
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- 229940073455 tetraethylammonium hydroxide Drugs 0.000 title claims abstract description 39
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229960003750 ethyl chloride Drugs 0.000 claims abstract description 31
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 22
- 239000001301 oxygen Substances 0.000 claims abstract description 22
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 22
- YMBCJWGVCUEGHA-UHFFFAOYSA-M tetraethylammonium chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC YMBCJWGVCUEGHA-UHFFFAOYSA-M 0.000 claims abstract description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 63
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 63
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 32
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 15
- 239000012498 ultrapure water Substances 0.000 claims description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 14
- 239000003011 anion exchange membrane Substances 0.000 claims description 14
- 238000005341 cation exchange Methods 0.000 claims description 14
- ULFQGKXWKFZMLH-UHFFFAOYSA-N iridium tantalum Chemical compound [Ta].[Ir] ULFQGKXWKFZMLH-UHFFFAOYSA-N 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 239000012528 membrane Substances 0.000 claims description 14
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- 239000010936 titanium Substances 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 2
- 230000006837 decompression Effects 0.000 claims description 2
- 229910001416 lithium ion Inorganic materials 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 32
- 238000000034 method Methods 0.000 abstract description 8
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 5
- 239000006227 byproduct Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000007086 side reaction Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 13
- 238000001816 cooling Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003444 phase transfer catalyst Substances 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 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
- 229910008062 Si-SiO2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910006403 Si—SiO2 Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000005459 micromachining Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- ZMANZCXQSJIPKH-UHFFFAOYSA-O triethylammonium ion Chemical compound CC[NH+](CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-O 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/01—Products
- C25B3/09—Nitrogen containing compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/04—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups
- C07C209/06—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms
- C07C209/12—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms with formation of quaternary ammonium compounds
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/01—Products
- C25B3/07—Oxygen containing compounds
Abstract
The invention discloses a preparation method of energy-saving tetraethyl ammonium hydroxide with high production efficiency, which sequentially comprises the following steps: oxygen is removed, chloroethane is introduced and electrolysis is carried out. The preparation method of the energy-saving tetraethyl ammonium hydroxide with high production efficiency; compared with the traditional production process, the nitrogen is used for pressurizing, the production efficiency of tetraethylammonium chloride can be higher, the net value is easy to separate, byproducts are less, the production period is short, the equipment investment and the energy consumption are relatively less, the side reaction in the preparation process is small, the purity of the product is higher, the preparation process is simple, and the method is suitable for industrial large-scale production, so that the requirement of tetraethylammonium hydroxide is met, and the environmental pollution is reduced.
Description
Technical Field
The invention relates to the technical field of compound preparation, in particular to a preparation method of energy-saving tetraethylammonium hydroxide with high production efficiency.
Background
Tetraethyl ammonium hydroxide is a common chemical product in the market, has wide application, and is mainly used as a template agent, a phase transfer catalyst, an impurity removing agent in the petroleum industry and the like. Tetraethyl ammonium hydroxide is an indispensable basic intermediate for promoting the development of industries such as organic synthesis, medicine, petroleum and the like.
Tetraethyl ammonium hydroxide is an organic alkali and is a catalyst in the synthesis of silicone rubber, silicone resin, silicone oil and other organic silicon products. It is widely used in the electronic industry as cleaning, etching and polishing reagents of integrated circuit boards and also used for anisotropic etching of Si-SiO2 interface in semiconductor micromachining technology. In addition, the catalyst can also be used as a phase transfer catalyst, a template agent for molecular sieve synthesis, a cleaning agent, a petroleum industry impurity removing agent and the like.
The traditional production method of tetraethyl ammonium hydroxide generally adopts methods such as a silver oxide method, an alkali replacement method and an ion exchange resin method, and has the problems of high production cost, poor product quality, difficulty in realizing large-scale production and the like. In addition, waste water containing quaternary ammonium compounds, which is difficult to treat, is generated during the preparation process, causing adverse environmental effects. Under the national large environment with higher and higher environmental requirements, the traditional TEAH production method is difficult to meet the requirements.
However, the existing method for preparing tetraethyl ammonium hydroxide has the following disadvantages in use, such as;
the preparation process has the disadvantages of insufficient energy conservation, energy waste, low production efficiency, inconvenient preparation, inconvenient operation and difficult large-scale production.
Therefore, we propose a method for preparing tetraethylammonium hydroxide with high production efficiency and energy saving, so as to solve the problems mentioned above.
Disclosure of Invention
The invention aims to provide a preparation method of energy-saving tetraethylammonium hydroxide with high production efficiency, which aims to solve the problems of insufficient energy conservation, relatively waste of energy, low production efficiency, inconvenience in preparation, inconvenience in operation and difficulty in large-scale production in the preparation process of the tetraethylammonium hydroxide in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: the preparation method of the energy-saving tetraethyl ammonium hydroxide with high production efficiency comprises the following steps of mixing raw materials, wherein the acetonitrile solution, triethylamine, ethyl chloride and inert gas sequentially comprise the following steps:
(1) preparing an electrolysis device: the anion exchange membrane 1, the cation exchange membrane 1, the anion exchange membrane 2 and the cation exchange membrane 2 form a cathode chamber, an anode chamber, a product chamber, an acid liquid chamber and a feed liquid chamber.
(2) Removing oxygen: adding triethylamine and acetonitrile solution into the high-pressure reaction kettle, and then passing nitrogen to remove oxygen in the high-pressure reaction kettle, so that the oxygen content of air in the container is less than one percent by volume percentage, thereby preventing oxidation in the reaction process.
(3) Introducing chloroethane: introducing a certain amount of chloroethane into the high-pressure reaction kettle, continuously adding nitrogen, pressurizing the chloroethane, stirring the chloroethane at a constant temperature, cooling the chloroethane to separate out a crystalline product tetraethylammonium chloride, and adding ultrapure water to easily dilute the crystalline tetraethylammonium chloride.
(4) Electrolysis: the solution in the cathode chamber is sodium hydroxide solution, the solution in the anode chamber is sulfuric acid, then the corresponding solution is added into the other three chambers, then air is discharged, the solution is added, the concentration of the solution in each chamber is kept at the temperature, the temperature is kept between 25 ℃ and 35 ℃, ultrapure water is introduced into the product chamber, the cathode and anode are all iridium-tantalum coating titanium electrodes, then tetraethylammonium hydroxide is added into the cathode chamber, tetraethylammonium chloride is added into the anode chamber, electrolysis is carried out, and then decompression and concentration are carried out to obtain the cathode-anode lithium ion battery.
Preferably, the temperature in the step (2) is required to be heated to 110-160 ℃.
Preferably, the stirring time in the step (2) is 3-8 h.
Preferably, in the step (3), the solution in the cathode chamber is sodium hydroxide solution, and the solution in the anode chamber is sulfuric acid.
Preferably, the mass fraction of the sodium hydroxide solution in the step (3) is 10-20%, and the mass fraction of the sulfuric acid is 10-20%.
Preferably, the experimental water is ultrapure water.
Preferably, the molar ratio between the acetonitrile solution, ethyl chloride and triethylamine is 1.8: 1.6:1.1.
Preferably, the electrode of the invention is an iridium tantalum coating titanium electrode.
Preferably, the temperature is maintained between 25-35 ℃ without heating.
Compared with the prior art, the invention has the beneficial effects that: the preparation method of the energy-saving tetraethyl ammonium hydroxide with high production efficiency;
compared with the traditional production process, the nitrogen is used for pressurizing, the production efficiency of tetraethylammonium chloride can be higher, the net value is easy to separate, byproducts are less, the production period is short, the equipment investment and the energy consumption are relatively less, the side reaction in the preparation process is small, the purity of the product is higher, the preparation process is simple, and the method is suitable for industrial large-scale production, so that the requirement of tetraethylammonium hydroxide is met, and the environmental pollution is reduced.
The iridium-tantalum coating titanium electrode is adopted, so that the acid resistance and the alkali resistance are enhanced, the production efficiency is better, the production cost is reduced, and the impurity concentration is reduced.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
The invention provides a technical scheme that: the preparation method of the energy-saving tetraethyl ammonium hydroxide with high production efficiency comprises the following steps of mixing raw materials, wherein the acetonitrile solution, triethylamine, ethyl chloride and inert gas sequentially comprise the following steps:
(1) preparing an electrolysis device: the anion exchange membrane 1, the cation exchange membrane 1, the anion exchange membrane 2 and the cation exchange membrane 2 form a cathode chamber, an anode chamber, a product chamber, an acid liquid chamber and a feed liquid chamber.
(2) Removing oxygen: adding triethylamine and acetonitrile solution into the high-pressure reaction kettle, and then passing nitrogen to remove oxygen in the high-pressure reaction kettle, so that the oxygen content of air in the container is less than one percent by volume percentage, thereby preventing oxidation in the reaction process.
(3) Introducing chloroethane: then adding a certain amount of chloroethane into the product obtained in the step (1), wherein the molar mass ratio of the acetonitrile solution to the chloroethane to the triethylamine is 1.8:1.6:1.1, then heating the mixture until the temperature of the mixture reaches 110 ℃, then stirring the mixture at a constant temperature for 3 hours, then cooling the mixture to separate out a crystalline product of tetraethylammonium chloride, and then adding ultrapure water to easily dilute the crystalline tetraethylammonium chloride.
(4) Electrolysis: the solution in the cathode chamber is sodium hydroxide solution, the mass fraction of the sodium hydroxide solution is 10%, the solution in the anode chamber is sulfuric acid, the mass fraction of the sulfuric acid is 10%, then the other three chambers are added with corresponding solutions, then air is discharged, the air is added, the solution concentration in each chamber is kept at the temperature, the temperature is kept between 25 ℃, ultrapure water is introduced into the product chamber, the cathode and the anode are all iridium-tantalum coating titanium electrodes, then tetraethylammonium hydroxide is added into the cathode chamber, tetraethylammonium chloride is added into the anode chamber, electrolysis is carried out, and then reduced pressure concentration is carried out to obtain the iridium-tantalum coated titanium anode.
Example two
The invention provides a technical scheme that: the preparation method of the energy-saving tetraethyl ammonium hydroxide with high production efficiency comprises the following steps of mixing raw materials, wherein the acetonitrile solution, triethylamine, ethyl chloride and inert gas sequentially comprise the following steps:
(1) preparing an electrolysis device: the anion exchange membrane 1, the cation exchange membrane 1, the anion exchange membrane 2 and the cation exchange membrane 2 form a cathode chamber, an anode chamber, a product chamber, an acid liquid chamber and a feed liquid chamber.
(2) Removing oxygen: adding triethylamine and acetonitrile solution into the high-pressure reaction kettle, and then passing nitrogen to remove oxygen in the high-pressure reaction kettle, so that the oxygen content of air in the container is less than one percent by volume percentage, thereby preventing oxidation in the reaction process.
(3) Introducing chloroethane: then adding a certain amount of chloroethane into the product obtained in the step (1), wherein the molar mass ratio of the acetonitrile solution to the chloroethane to the triethylamine is 1.8:1.6:1.1, then heating the mixture until the temperature reaches 130 ℃, then stirring the mixture at a constant temperature for 5 hours, then cooling the mixture to separate out a crystalline product of tetraethylammonium chloride, and then adding ultrapure water to easily dilute the crystalline tetraethylammonium chloride.
(4) Electrolysis: the solution in the cathode chamber is sodium hydroxide solution, the mass fraction of the sodium hydroxide solution is 14%, the solution in the anode chamber is sulfuric acid, the mass fraction of the sulfuric acid is 14%, then the other three chambers are added with corresponding solutions, then air is discharged, the air is added, the solution concentration in each chamber is kept at 26 ℃, ultrapure water is introduced into the product chamber, the cathode and the anode are all iridium-tantalum coating titanium electrodes, then tetraethylammonium hydroxide is added into the cathode chamber, tetraethylammonium chloride is added into the anode chamber, electrolysis is carried out, and then reduced pressure concentration is carried out to obtain the iridium-tantalum coated titanium anode.
EXAMPLE III
The invention provides a technical scheme that: the preparation method of the energy-saving tetraethyl ammonium hydroxide with high production efficiency comprises the following steps of mixing raw materials, wherein the acetonitrile solution, triethylamine, ethyl chloride and inert gas sequentially comprise the following steps:
(1) preparing an electrolysis device: the anion exchange membrane 1, the cation exchange membrane 1, the anion exchange membrane 2 and the cation exchange membrane 2 form a cathode chamber, an anode chamber, a product chamber, an acid liquid chamber and a feed liquid chamber.
(2) Removing oxygen: adding triethylamine and acetonitrile solution into the high-pressure reaction kettle, and then passing nitrogen to remove oxygen in the high-pressure reaction kettle, so that the oxygen content of air in the container is less than one percent by volume percentage, thereby preventing oxidation in the reaction process.
(3) Introducing chloroethane: then adding a certain amount of chloroethane into the product obtained in the step (1), wherein the molar mass ratio of the acetonitrile solution to the chloroethane to the triethylamine is 1.8:1.6:1.1, then heating the mixture until the temperature reaches 140 ℃, then stirring the mixture at a constant temperature for 6 hours, then cooling the mixture to separate out a crystalline product of tetraethylammonium chloride, and then adding ultrapure water to easily dilute the crystalline tetraethylammonium chloride.
(4) Electrolysis: the solution in the cathode chamber is sodium hydroxide solution, the mass fraction of the sodium hydroxide solution is 16%, the solution in the anode chamber is sulfuric acid, the mass fraction of the sulfuric acid is 16%, then the other three chambers are added with corresponding solutions, then air is discharged, the air is added, the solution concentration in each chamber is kept at 28 ℃, ultrapure water is introduced into the product chamber, the cathode and the anode are all iridium-tantalum coating titanium electrodes, then tetraethylammonium hydroxide is added into the cathode chamber, tetraethylammonium chloride is added into the anode chamber, electrolysis is carried out, and then reduced pressure concentration is carried out to obtain the iridium-tantalum coated titanium anode material.
Example four
The invention provides a technical scheme that: the preparation method of the energy-saving tetraethyl ammonium hydroxide with high production efficiency comprises the following steps of mixing raw materials, wherein the acetonitrile solution, triethylamine, ethyl chloride and inert gas sequentially comprise the following steps:
(1) preparing an electrolysis device: the anion exchange membrane 1, the cation exchange membrane 1, the anion exchange membrane 2 and the cation exchange membrane 2 form a cathode chamber, an anode chamber, a product chamber, an acid liquid chamber and a feed liquid chamber.
(2) Removing oxygen: adding triethylamine and acetonitrile solution into the high-pressure reaction kettle, and then passing nitrogen to remove oxygen in the high-pressure reaction kettle, so that the oxygen content of air in the container is less than one percent by volume percentage, thereby preventing oxidation in the reaction process.
(3) Introducing chloroethane: then adding a certain amount of chloroethane into the product obtained in the step (1), wherein the molar mass ratio of the acetonitrile solution to the chloroethane to the triethylamine is 1.8:1.6:1.1, then heating the mixture until the temperature reaches 150 ℃, then stirring the mixture at a constant temperature for 7 hours, then cooling the mixture to separate out a crystalline product of tetraethylammonium chloride, and then adding ultrapure water to easily dilute the crystalline tetraethylammonium chloride.
(4) Electrolysis: the solution in the cathode chamber is sodium hydroxide solution, the mass fraction of the sodium hydroxide solution is 18%, the solution in the anode chamber is sulfuric acid, the mass fraction of the sulfuric acid is 18%, then the other three chambers are added with corresponding solutions, then air is discharged, the air is added, the solution concentration in each chamber is kept at the temperature, the temperature is kept between 30 ℃, ultrapure water is introduced into the product chamber, the cathode and the anode are all iridium-tantalum coating titanium electrodes, then tetraethylammonium hydroxide is added into the cathode chamber, tetraethylammonium chloride is added into the anode chamber, electrolysis is carried out, and then reduced pressure concentration is carried out to obtain the product.
EXAMPLE five
The invention provides a technical scheme that: the preparation method of the energy-saving tetraethyl ammonium hydroxide with high production efficiency comprises the following steps of mixing raw materials, wherein the acetonitrile solution, triethylamine, ethyl chloride and inert gas sequentially comprise the following steps:
(1) preparing an electrolysis device: the anion exchange membrane 1, the cation exchange membrane 1, the anion exchange membrane 2 and the cation exchange membrane 2 form a cathode chamber, an anode chamber, a product chamber, an acid liquid chamber and a feed liquid chamber.
(2) Removing oxygen: adding triethylamine and acetonitrile solution into the high-pressure reaction kettle, and then passing nitrogen to remove oxygen in the high-pressure reaction kettle, so that the oxygen content of air in the container is less than one percent by volume percentage, thereby preventing oxidation in the reaction process.
(3) Introducing chloroethane: then adding a certain amount of ethyl chloride into the product obtained in the step (1), wherein the molar mass ratio of the acetonitrile solution to the ethyl chloride to the triethylamine is 1.8:1.6:1.1, heating the product until the temperature reaches 160 ℃, then stirring the product at constant temperature for 8 hours, then cooling the product to separate out a crystalline product of tetraethylammonium chloride, and then adding ultrapure water to easily dilute the crystalline tetraethylammonium chloride.
(4) Electrolysis: the solution in the cathode chamber is sodium hydroxide solution, the mass fraction of the sodium hydroxide solution is 20%, the solution in the anode chamber is sulfuric acid, the mass fraction of the sulfuric acid is 20%, then the other three chambers are added with corresponding solutions, then air is discharged, the air is added, the solution concentration in each chamber is kept at the temperature, the temperature is kept between 35 ℃, ultrapure water is introduced into the product chamber, the cathode and the anode are all iridium-tantalum coating titanium electrodes, then tetraethylammonium hydroxide is added into the cathode chamber, tetraethylammonium chloride is added into the anode chamber, electrolysis is carried out, and then reduced pressure concentration is carried out to obtain the iridium-tantalum coated titanium anode.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (9)
1. The preparation method of the energy-saving tetraethylammonium hydroxide with high production efficiency is characterized by comprising the following steps: the mixed raw materials comprise the following components of acetonitrile solution, triethylamine, chloroethane and inert gas, and sequentially comprise the following steps:
(1) preparing an electrolysis device: an anion exchange membrane 1, a cation exchange membrane 1, an anion exchange membrane 2 and a cation exchange membrane 2, thereby forming a cathode chamber, an anode chamber, a product chamber, an acid liquid chamber and a material liquid chamber,
(2) removing oxygen: adding triethylamine and acetonitrile solution into the high-pressure reaction kettle, and then passing nitrogen to remove oxygen in the high-pressure reaction kettle, so that the oxygen content of air in the container is less than one percent by volume percentage, thereby preventing oxidation in the reaction process.
(3) Introducing chloroethane: the solution in the cathode chamber is sodium hydroxide solution, the solution in the anode chamber is sulfuric acid, then the corresponding solution is added into the other three chambers, then air is discharged, the solution is added, the concentration of the solution in each chamber is kept at the temperature, the temperature is kept between 25 ℃ and 35 ℃, ultrapure water is introduced into the product chamber, the cathode and anode are all iridium-tantalum coating titanium electrodes, then tetraethylammonium hydroxide is added into the cathode chamber, tetraethylammonium chloride is added into the anode chamber, electrolysis is carried out, and then decompression and concentration are carried out to obtain the cathode-anode lithium ion battery.
(4) Electrolysis: adding tetraethylammonium hydroxide into the cathode chamber, adding tetraethylammonium chloride into the anode chamber, then electrolyzing, and then concentrating under reduced pressure to obtain a finished product.
2. The preparation method of the energy-saving tetraethylammonium hydroxide with high production efficiency according to claim 1 is characterized in that: the temperature in the step (2) needs to be heated to 110-160 ℃.
3. The preparation method of the energy-saving tetraethylammonium hydroxide with high production efficiency according to claim 1 is characterized in that: the stirring time in the step (2) is 3-8 h.
4. The preparation method of the energy-saving tetraethylammonium hydroxide with high production efficiency according to claim 1 is characterized in that: and (3) the solution in the cathode chamber in the step (3) is sodium hydroxide solution, and the solution in the anode chamber is sulfuric acid.
5. The preparation method of the energy-saving tetraethylammonium hydroxide with high production efficiency according to claim 1 is characterized in that: in the step (3), the mass fraction of the sodium hydroxide solution is 10-20%, and the mass fraction of the sulfuric acid is 10-20%.
6. The preparation method of the energy-saving tetraethylammonium hydroxide with high production efficiency according to claim 1 is characterized in that: the experimental water is ultrapure water.
7. The preparation method of the energy-saving tetraethylammonium hydroxide with high production efficiency according to claim 1 is characterized in that: the molar ratio of the acetonitrile solution to the ethyl chloride to the triethylamine is 1.8: 1.6:1.1.
8. The preparation method of the energy-saving tetraethylammonium hydroxide with high production efficiency according to claim 1 is characterized in that: the electrode is an iridium tantalum coating titanium electrode.
9. The preparation method of the energy-saving tetraethylammonium hydroxide with high production efficiency according to claim 1 is characterized in that: the temperature is maintained between 25-35 ℃ when no heating is required.
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| CN202111094977.0A CN113981476A (en) | 2021-09-17 | 2021-09-17 | Preparation method of energy-saving tetraethylammonium hydroxide with high production efficiency |
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