CN208532944U - A kind of equipment of continuity method production tetramethylammonium hydroxide - Google Patents
A kind of equipment of continuity method production tetramethylammonium hydroxide Download PDFInfo
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- CN208532944U CN208532944U CN201820771074.9U CN201820771074U CN208532944U CN 208532944 U CN208532944 U CN 208532944U CN 201820771074 U CN201820771074 U CN 201820771074U CN 208532944 U CN208532944 U CN 208532944U
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Abstract
The utility model provides a kind of equipment of continuity method production tetramethylammonium hydroxide.It is related to tetramethylammonium hydroxide production technical field, using the cell construction of two Room of a film;Anode part, which supplements anolyte by anolyte pans, keeps anode chamber's Anodic liquid concentration amplitude of variation in electrolytic process small.Catholyte tetramethylammonium hydroxide concentration is concentrated to the ability of shutting off hydroxy by nanofiltration device, using nanofiltration membrane in cathode portion, controls concentration ratio, dope enters products pot, and penetrating fluid enters catholyte.It is that tetramethylammonium hydroxide concentration amplitude of variation is small in catholyte.Technology and equipment equipment provided by the utility model is simple, reactor occupied area is small, equipment investment is small, and keep electrolytic process Anodic liquid and cathode liquid concentration amplitude of variation small by the allotment of anolyte pans and catholyte nano filter membrance device, process stabilizing, it is small to ion membrane damage, be conducive to the service life for increasing film.
Description
Technical field
The utility model relates to tetramethylammonium hydroxide production technical fields more particularly to a kind of continuity method to produce tetramethyl
The equipment of ammonium hydroxide.
Background technique
Tetramethylammonium hydroxide is a kind of important organic base, it has, and there are two types of characteristics: (1) decomposition temperature is low, after decomposition
Become gas, noresidue;It (2) is organic alkali in itself, alkalinity is strong, and non-metallic ion, the above characteristic makes it in electronic manufacture
Industry has important application.In electronic manufacturing industry, it is desirable that tetramethylammonium hydroxide impurity metal ion and anion are miscellaneous
Matter content is low, and if single metal ionic impurity is lower than 1ppb, anionic impurity ion is lower than 50ppb.
The method of production tetramethylammonium hydroxide is mainly electrolysis method at present.Two steps are divided to be made: first step tetramethyl ammonium
Synthesis;Second step converts final products tetramethylammonium hydroxide for tetramethyl ammonium by the method for electrolysis with ion-exchange film.Four
Methyl ammonium salt can there are many, such as tetramethyl ammonium chloride, tetramethyl ammonium carbonate, tetramethyl ammonium nitrate etc..Wherein tetramethyl carbonic acid
Ammonium is the tetramethyl ammonium salt of most mainstream.
Tetramethyl ammonium carbonate is reacted in methyl alcohol by trimethylamine and dimethyl carbonate generates tetramethyl carbonic acid mono-methyl, passes through
Hydrolysis generates tetramethyl ammonium carbonate and methanol.
Then pass through electrolysis with ion-exchange film in a cell using tetramethyl ammonium carbonate as raw material and tetramethylammonium hydroxide is made.
CN01104629.5, CN03106227.X, CN101597763A, CN102206832A use ion membrane electrolytic process
Obtain tetramethylammonium hydroxide.Above method catholyte in electrolytic process uses water or dilute tetramethylammonium hydroxide, is being electrolysed
Concentration of electrolyte variation greatly, not only influences properties of product but also reduces membrane life, increase production cost in the process.
Utility model content
It is above-mentioned to solve the purpose of this utility model is to provide a kind of equipment of continuity method production tetramethylammonium hydroxide
Technical problem.
The utility model using following technical scheme in order to solve the above technical problems, realized:
It is as follows that the utility model provides technology and equipment:
A kind of equipment of continuity method production tetramethylammonium hydroxide, it is characterised in that: including electrolytic cell, electrolyte bath is logical
It crosses cation-exchange membrane and electrolytic cell is separated into anode chamber and cathode chamber two parts,
Anode chamber part is sequentially connected anolyte pans, anolyte raw material tank by pipeline, and pump, institute are equipped on pipeline
It states the raw material in anolyte raw material tank and is unidirectionally pumped into anolyte pans, the segment anode liquid in anode chamber passes through a pipeline pump
Enter and deployed in anolyte pans, the anolyte of deployed concentration passes through another pipeline again and is pumped into anolyte pans
Anode chamber controls stabilization of Anodic liquid concentration in anode chamber's in electrolytic process;
Cathode chamber part is sequentially connected nanofiltration device, products pot by pipeline, and pump is also equipped on the pipeline of the part, yin
Pole room and nanofiltration device are by two piping connections, wherein the indoor catholyte of cathode is pumped into nanofiltration device by a pipeline, benefit
Concentration with the nanofiltration membrane of nanofiltration device to tetramethylammonium hydroxide in the ability of shutting off hydroxy concentration catholyte, control concentration
Ratio, concentration are pumped into products pot after reaching product design;The penetrating fluid part that nanofiltration device nanofiltration generates passes through another pipeline
It is pumped into cathode chamber, to guarantee that the variation of tetramethylammonium hydroxide concentration is small in catholyte.
Preferably, the anolyte pans external water pipe, for supplementing water.
Utilize the method for the continuity method production tetramethylammonium hydroxide of above equipment, it is characterised in that: tetramethyl ammonium carbonate
For raw material, the dope in anolyte raw material tank is unidirectionally pumped into anolyte pans, and the segment anode liquid in anode chamber passes through one
Pipeline is pumped into anolyte pans and is deployed, and the anolyte of deployed concentration passes through another pipe again in anolyte pans
Road is pumped into anode chamber, controls stabilization of Anodic liquid concentration in anode chamber's in electrolytic process;
The indoor catholyte of cathode is pumped into nanofiltration device, dense to the ability of shutting off hydroxy using the nanofiltration membrane of nanofiltration device
The concentration of tetramethylammonium hydroxide in contracting catholyte, controls concentration ratio, and concentration is pumped into products pot after reaching product design;Nanofiltration
The penetrating fluid part that device nanofiltration generates is pumped into cathode chamber, to guarantee that the variation of tetramethylammonium hydroxide concentration is small in catholyte.
Preferably, the concentration of raw material tetramethyl ammonium carbonate is 50-65%.
Preferably, anode chamber's Anodic liquid concentration is between 20-30%.
Preferably, tetramethylammonium hydroxide product design is in 10-18% in cathode chamber.
Preferably, tetramethyl ammonium carbonate is raw material, tetramethyl ammonium carbonate concentration is 65% in anolyte head tank, starting
Stage, allotment tetramethyl ammonium carbonate concentration was 35% by the ratio of control raw material and water in anolyte pans, then will
This solution injects anode chamber, is electrolysed, and as electrolysis carries out, anode solution concentration is reduced, and is at this time pumped into segment anode liquid
Anolyte pans, in conjunction in anolyte head tank raw material and water make tetramethyl ammonium carbonate concentration in anolyte pans
35%, this solution is then supplemented to anode chamber, is so recycled, keeps the anode solution concentration in anode chamber between 25-30%;
It carries out tetramethylammonium hydroxide concentration with electrolysis in cathode chamber constantly to rise, when concentration rises to 15-18%, catholyte, which is pumped into, to be received
Device is filtered, shuts off to achieve the purpose that concentrate to hydroxyl by the nanofiltration membrane of nanofiltration device, when dope side in nanofiltration device
Tetramethylammonium hydroxide concentration when reaching 20-25%, be pumped into products pot;Penetrating fluid concentration 11-13%, part in nanofiltration device
Penetrating fluid is pumped into cathode chamber, so recycles, and makes in cathode chamber tetramethylammonium hydroxide product design between 11-18%;Product
It is detected by ICP-MS, single metal ion is lower than 1ppb.
The utility model provides a kind of device and method of continuous production tetramethylammonium hydroxide.Equipment uses a film two
The cell construction of room;Anode part, which supplements anolyte by anolyte pans, had been electrolysed anode chamber's Anodic liquid concentration
Amplitude of variation is small in journey.Catholyte four is concentrated to the ability of shutting off hydroxy by nanofiltration device, using nanofiltration membrane in cathode portion
Ammonium hydroxide concentration controls concentration ratio, and dope enters products pot, and penetrating fluid enters catholyte.Make tetramethyl in catholyte
Base ammonium hydroxide concentration amplitude of variation is small.
The beneficial effects of the utility model are:
Technology and equipment equipment provided by the utility model is simple, and reactor occupied area is small, and equipment investment is small, Er Qietong
The allotment and catholyte nano filter membrance device for crossing anolyte pans make electrolytic process Anodic liquid and cathode liquid concentration amplitude of variation
Small, process stabilizing is small to ion membrane damage, is conducive to the service life for increasing film.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the utility model;
Appended drawing reference: 1- anolyte raw material tank;2- pump;3- anolyte pans;4- electrolytic cell;5- products pot;6- nanofiltration
Device;The anode chamber 41-;42- cathode chamber.
Specific embodiment
In order to be easy to understand the technical means, creative features, achievement of purpose, and effectiveness of the utility model, under
The utility model is further described in face with specific embodiments and the drawings, but following embodiments are only the excellent of the utility model
Embodiment is selected, and not all.Based on the implementation example in the implementation mode, those skilled in the art are not making creative work
Under the premise of obtained other embodiments, belong to the protection scope of the utility model.
Specific embodiment of the utility model is described with reference to the accompanying drawing.
As shown in Figure 1, a kind of equipment of continuity method production tetramethylammonium hydroxide, including electrolytic cell 4, inside electrolytic cell 4
Electrolytic cell is separated into 42 two parts of anode chamber 41 and cathode chamber by cation-exchange membrane,
41 part of anode chamber is sequentially connected anolyte pans 3, anolyte raw material tank 1 by pipeline, is equipped on pipeline
2 are pumped, the raw material in anolyte raw material tank 1 is unidirectionally pumped into anolyte pans 3, and the segment anode liquid in anode chamber 41 passes through one
Pipeline is pumped into anolyte pans 3 and is deployed, and the anolyte of deployed concentration passes through another again in anolyte pans 3
Pipeline is pumped into anode chamber 41, controls stabilization of the 41 Anodic liquid concentration of anode chamber in electrolytic process;
42 part of cathode chamber is sequentially connected nanofiltration device 6, products pot 5 by pipeline, is also equipped on the pipeline of the part
Pump 2, cathode chamber 42 and nanofiltration device 6 are by two piping connections, wherein the catholyte in cathode chamber 42 is pumped by a pipeline
Nanofiltration device 6, using the nanofiltration membrane of nanofiltration device 6 to tetramethylammonium hydroxide in the ability of shutting off hydroxy concentration catholyte
Concentration, controls concentration ratio, and concentration is pumped into products pot 5 after reaching product design;The penetrating fluid part that 6 nanofiltration of nanofiltration device generates
It is pumped into cathode chamber 42 by another pipeline, to guarantee that the variation of tetramethylammonium hydroxide concentration is small in catholyte.
The method of continuity method production tetramethylammonium hydroxide:
Embodiment 1
Tetramethyl ammonium carbonate is raw material, and tetramethyl ammonium carbonate concentration is 65% in anolyte head tank, and initial phase is in sun
By the ratio of control raw material and water in the liquid pans of pole, allotment tetramethyl ammonium carbonate concentration is 35%, then infuses this solution
Enter anode chamber, be electrolysed, as electrolysis carries out, anode solution concentration is reduced, and at this time enters segment anode liquid pump into anolyte
Between tank, in conjunction in anolyte head tank raw material and water make tetramethyl ammonium carbonate concentration 35% in anolyte pans, then
This solution is supplemented to anode chamber, is so recycled, keeps the anode solution concentration in anode chamber between 25-30%.In cathode chamber
It carries out tetramethylammonium hydroxide concentration with electrolysis constantly to rise, when concentration rises to 18%, catholyte is pumped into nanofiltration device, passes through
The nanofiltration membrane of nanofiltration device shuts off hydroxyl to achieve the purpose that concentrate, when the tetramethyl hydrogen-oxygen of dope side in nanofiltration device
When change ammonium concentration reaches 25%, it is pumped into products pot.Penetrating fluid concentration about 13% in nanofiltration device, partial penetration liquid pump enter cathode
Room so recycles, and makes in cathode chamber tetramethylammonium hydroxide product design between 13-18%.Product is detected by ICP-MS,
Single metal ion is lower than 1ppb.
Embodiment 2
Tetramethyl ammonium carbonate is raw material, and tetramethyl ammonium carbonate concentration is 65% in anolyte head tank, and initial phase is in sun
By the ratio of control raw material and water in the liquid pans of pole, allotment tetramethyl ammonium carbonate concentration is 35%, then infuses this solution
Enter anode chamber, be electrolysed, as electrolysis carries out, anode solution concentration is reduced, and at this time enters segment anode liquid pump into anolyte
Between tank, in conjunction in anolyte head tank raw material and water make tetramethyl ammonium carbonate concentration 35% in anolyte pans, then
This solution is supplemented to anode chamber, is so recycled, keeps the anode solution concentration in anode chamber between 25-30%.In cathode chamber
It carries out tetramethylammonium hydroxide concentration with electrolysis constantly to rise, when concentration rises to 15%, catholyte is pumped into nanofiltration device, passes through
The nanofiltration membrane of nanofiltration device shuts off hydroxyl to achieve the purpose that concentrate, when the tetramethyl hydrogen-oxygen of dope side in nanofiltration device
When change ammonium concentration reaches 20%, it is pumped into products pot.Penetrating fluid concentration about 11% in nanofiltration device, partial penetration liquid pump enter cathode
Room so recycles, and makes in cathode chamber tetramethylammonium hydroxide product design between 11-15%.Product is detected by ICP-MS,
Single metal ion is lower than 1ppb.
Basic principles, main features, and advantages of the present invention has been shown and described above.Current row
The technical staff of industry is described in above embodiments and description it should be appreciated that the present utility model is not limited to the above embodiments
Be only the utility model preference, be not intended to limit the utility model, do not departing from the spirit and scope of the utility model
Under the premise of, the utility model also has various changes and improvements, these changes and improvements both fall within claimed it is practical
In novel range.The protection scope of the present invention is defined by the appended claims and their equivalents.
Claims (2)
1. a kind of equipment of continuity method production tetramethylammonium hydroxide, it is characterised in that: including electrolytic cell, electrolyte bath passes through
Electrolytic cell is separated into anode chamber and cathode chamber two parts by cation-exchange membrane,
Anode chamber part is sequentially connected anolyte pans, anolyte raw material tank by pipeline, and pump, the sun are equipped on pipeline
Raw material in the liquid raw material tank of pole is unidirectionally pumped into anolyte pans, and the segment anode liquid in anode chamber is pumped into sun by a pipeline
It is deployed in the liquid pans of pole, the anolyte of deployed concentration passes through another pipeline again and is pumped into anode in anolyte pans
Room controls stabilization of Anodic liquid concentration in anode chamber's in electrolytic process;
Cathode chamber part is sequentially connected nanofiltration device, products pot by pipeline, is also equipped with pump, cathode chamber on the pipeline of the part
With nanofiltration device by two piping connections, wherein the indoor catholyte of cathode is pumped into nanofiltration device by a pipeline, using receiving
The nanofiltration membrane of device is filtered to the concentration of tetramethylammonium hydroxide in the ability of shutting off hydroxy concentration catholyte, controls cocnentration factor
Example, concentration are pumped into products pot after reaching product design;The penetrating fluid part that nanofiltration device nanofiltration generates passes through another pipeline pump
Enter cathode chamber, to guarantee that the variation of tetramethylammonium hydroxide concentration is small in catholyte.
2. the equipment of continuity method production tetramethylammonium hydroxide according to claim 1, it is characterised in that: the anolyte
Pans external water pipe, for supplementing water.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108396327A (en) * | 2018-05-23 | 2018-08-14 | 梁小朝 | A kind of device and method of continuity method production tetramethylammonium hydroxide |
CN110055551A (en) * | 2019-05-31 | 2019-07-26 | 中触媒新材料股份有限公司 | A kind of device and method that cavity block electrolysis method prepares tetra-alkyl ammonium hydroxide |
CN111962096A (en) * | 2020-08-13 | 2020-11-20 | 沧州信联化工有限公司 | Synthetic method and equipment for tetramethylammonium hydroxide |
-
2018
- 2018-05-23 CN CN201820771074.9U patent/CN208532944U/en active Active
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108396327A (en) * | 2018-05-23 | 2018-08-14 | 梁小朝 | A kind of device and method of continuity method production tetramethylammonium hydroxide |
CN108396327B (en) * | 2018-05-23 | 2024-04-09 | 柏川新材料科技(宁波)有限公司 | Equipment and method for producing tetramethyl ammonium hydroxide by continuous method |
CN110055551A (en) * | 2019-05-31 | 2019-07-26 | 中触媒新材料股份有限公司 | A kind of device and method that cavity block electrolysis method prepares tetra-alkyl ammonium hydroxide |
CN111962096A (en) * | 2020-08-13 | 2020-11-20 | 沧州信联化工有限公司 | Synthetic method and equipment for tetramethylammonium hydroxide |
CN111962096B (en) * | 2020-08-13 | 2021-12-10 | 沧州信联化工有限公司 | Synthetic method and equipment for tetramethylammonium hydroxide |
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Effective date of registration: 20220727 Address after: 315048 A1 on the first floor of plant 6, No. 96, hibiscus Road, high tech Zone, Ningbo, Zhejiang Province Patentee after: Baichuan new material technology (Ningbo) Co.,Ltd. Address before: 310006 No. 155 Dongxin Road, Xiacheng District, Hangzhou City, Zhejiang Province Patentee before: Liang Xiaochao Patentee before: Yao Haochuan |