CN104278288A - Method for preparing high-purity tetrabutyl ammonium hydroxide by continuous electrolysis - Google Patents
Method for preparing high-purity tetrabutyl ammonium hydroxide by continuous electrolysis Download PDFInfo
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- CN104278288A CN104278288A CN201410516813.6A CN201410516813A CN104278288A CN 104278288 A CN104278288 A CN 104278288A CN 201410516813 A CN201410516813 A CN 201410516813A CN 104278288 A CN104278288 A CN 104278288A
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Abstract
The invention relates to a method for preparing high-purity tetrabutyl ammonium hydroxide by continuous electrolysis, particularly relates to a method for preparing high-purity tetrabutyl ammonium hydroxide by using tetrabutyl ammonium bromide as a raw material and adopting a three-compartment bipolar membrane electrodialysis device, and belongs to the field of organic chemistry. The method is characterized by comprising the following step: by adopting the three-compartment bipolar membrane electrodialysis device, continuously preparing 5-20% tetrabutyl ammonium hydroxide by using a 15-35% tetrabutyl ammonium bromide aqueous solution as a raw material under the condition that the reaction temperature is 30-60 DEG C, the current density is 200-600A/m<2> and the flow rate of the raw materials is 500-2000L/h, wherein the concentration of bromine ions in the prepared tetrabutyl ammonium hydroxide is less than 100ppm. According to the method provided by the invention, the materials in the compartments are relatively constant in concentration, the temperature is relatively constant, an ionic membrane is not easy to swell or shrink, the membrane cost is saved, the current efficiency and the product conversion ratio are improved and the energy consumption is reduced, and moreover, the product quality is further improved. The method is suitable for industrial safe production on a large scale, clean in production process and free of discharge of wastewater and solid wastes.
Description
Technical field
The present invention relates to a kind of method that continuous electrolysis prepares high-purity TBAH, particularly the method for the high-purity TBAH of a kind of employing three compartment bipolar membrane electrodialysis device continuous production, belongs to organic chemistry filed.
Background technology
TBAH (TBAOH) is a kind of organic quaternary ammonium highly basic.TBAH is commonly used for organic synthesis reagent, tensio-active agent, phase-transfer catalyst, the cleaning reagent of electronic industry, polarographic analysis reagent.Wherein high-purity TBAH is mainly used for cleaning and the corrosion of chip, and its purity and cleanliness factor have very important impact to the yield rate of unicircuit, electrical property and reliability.High-purity TBAH has unique effect due to it, alternative tetramethyl-hydroxide money and tetraethyl-hydroxide is pressed, and as third generation micro-electronics chemicals by for more advanced 18 nano chips in future.Therefore, the method for the high-purity TBAH of research preparation is to promoting that the development of microelectronic industry has very important effect.
The preparation method of TBAH mainly contains silver suboxide method, potassium hydroxide method, electrolytic process, ion exchange method, organic acid 4-butyl ammonium Current Decomposition method, ionic membrane method etc.Patent CN102030665 disclose a kind of adopt chemical method prepare tetrabutylammonium hydroxide by technique.TBAH purity prepared by this method is not high, there is a large amount of negatively charged ion (being that main memory exists with bromide anion), is difficult to the requirement reaching microelectronics industry.Adopt anion exchange method can prepare the higher TBAH of purity, but exchange degree is generally maximum to 90%.East China University of Science Yang Jiao proposes the method that employing three Room two membrane electrolyser prepares high-purity TBAH, and this method is difficult to the continuous production realizing high-purity TBAH.
Summary of the invention
The object of the invention is to provide a kind of continuous electrolysis to prepare the method for high-purity TBAH, effectively overcome the shortcoming that in existing TBAH preparation technology products obtained therefrom, bromide ion concentration is higher, overcome simultaneously interval electrolysis TBAH purifying technique can not serialization, small serial production shortcoming, realize high-purity TBAH and produce in enormous quantities continuously.
A kind of continuous electrolysis of the present invention prepares the method for high-purity TBAH, and the technical scheme of employing is as follows:
the present invention adopts a kind of three compartment bipolar membrane electrodialysis devices (see accompanying drawing 1), and take Tetrabutyl amonium bromide as raw material, continuous electrolysis prepares high-purity TBAH that bromide ion concentration is less than 100 ppm, and concrete operations are as follows:
(1) three compartment type bipolar membrane electrodialysis devices are formed with 1 Bipolar Membrane, 1 cationic exchange membrane and 1 anion-exchange membrane; Three described compartments are made up of electrodialysis compartment in the middle of two pole liquid chambers and; Described intermediate chamber is made up of sour room, alkali room and salt room; Described three compartment type bipolar membrane electrodialysis devices divide poling liquid chamber 1, sour room 2, salt room 3, alkali room 4, pole liquid chamber 5 successively; Bipolar Membrane 6 is accompanied between pole liquid chamber 1 and sour room 2; Anionic membrane 7 is accompanied between acid room 2 and salt room 3; Cationic membrane 8 is accompanied between salt room 3 and alkali room 4; Bipolar Membrane 9 is accompanied between alkali room 4 and pole liquid chamber 5; In pole liquid chamber 1, insert positive plate 10, in pole liquid chamber 5, insert negative plate 11.
(2) in feedstock circulation tank 13, mass concentration is that 15% ~ 35%(unexplained reference is mass concentration, lower same) Tetrabutyl amonium bromide (TBABr) aqueous solution, squeeze into salt room 3 through pump 14, control raw material flow rate; Positively charged ion TBA is produced in TBABr hydrolysis
+and negatively charged ion Br
-; Opening power 12, controls current density, under osmosis and electric field action, and positively charged ion TBA
+alkali room 4 is entered, negatively charged ion Br through cationic membrane 8
-sour room 2 is entered through anionic membrane; The TBABr do not permeated, through recycle pump 28, mixes with the TBABr aqueous solution 21, and incoming stock circulation tank 13 reuses.
(3) ultrapure water (H
2o) 17 squeeze in alkali room 4 through pump 18, H
2o electrolysis generates positively charged ion H
+and negatively charged ion OH
-; Positively charged ion H
+pole liquid chamber 5 is entered through Bipolar Membrane 9 under electric field action; Negatively charged ion OH
-remain in alkali room 4, with the TBA entering alkali room 4 from salt room 3
+form TBAOH; Through pump 24 from discharge port 25 discharging.
(4) ultrapure water 15 is squeezed in sour room 2 through pump 16, and water electrolysis generates positively charged ion H
+and negatively charged ion OH
-; Negatively charged ion OH
-pole liquid chamber 1 is entered through Bipolar Membrane 6 under electric field action; Positively charged ion H
+remain in sour room 2, with the Br entering sour room 2 from salt room 3
-form HBr; Export from discharge port 23 through pump 22.
(5) the pole liquid in pole liquid chamber 1 recycles through recycle pump 19; The negatively charged ion OH of pole liquid chamber 1 is entered from sour room 2
-with Br
-, at a certain temperature, with positive plate effect, lose electronics and form O
2and Br
2, bring large quantity of air into through gas blower 26, by generated O
2with the micro-Br that infiltration is come
2discharge, through alkali liquor absorption from venting port 27.
(6) the pole liquid in pole liquid chamber 5 recycles through recycle pump 20; The positively charged ion H of pole liquid chamber 5 is entered from alkali room 4
+, with negative plate effect, obtain electronics and form H
2, the large quantity of air brought into gas blower 28, discharges from venting port 29.
Be mass concentration 15% ~ 35% tetrabutyl phosphonium bromide aqueous ammonium in head tank 13 described in step (2) in technique scheme, need, through treatment on ion exchange columns, to obtain high-purity raw.
The mass concentration of the TBABr aqueous solution 21 described in step (2) is greater than 15% ~ 35%.
Controlling raw material flow rate described in step (2) is 500 ~ 2000 L/h.
The current density controlling bipolar membrane electrodialysis device described in step (2) is 200 ~ 600 A/m
2.
It is 3 ~ 5% aqueous sulfuric acids that pole liquid in pole liquid chamber 5 described in pole liquid in pole liquid chamber 1 described in step (4) and step (5) is mass concentration.
In technique scheme, controlling temperature of reaction in preparation process is 30 ~ 60 DEG C.
In technique scheme, the TBAH mass concentration obtained is 5% ~ 20% aqueous solution.
In the high-purity TPAOH obtained in technique scheme, bromide ion concentration is less than 100 ppm.
The invention has the advantages that:
1. adopt continuous process, continuously feeding, continuous discharge, each material concentration relative constancy in bipolar membrane electrodialysis device compartment, temperature relative constancy, not easily there is the problem that swelling or contraction etc. affect service life of ion-exchange membrane and performance in ionic membrane, saves film cost, improve current efficiency and conversion rate of products, reduce energy consumption, also further increase product quality.
2. continuous processing preparation technology is convenient to adopt automatization, can reduce the generation of all kinds of security incident, is suitable for industrially scalable safety in production.
3, continuous processing electrolysis is cleansing preparation method of making, without waste water, solid-state castoff discharge.
Accompanying drawing explanation
Fig. 1 is three compartment bipolar membrane electrodialysis device schematic diagram of the present invention; 1. pole liquid chambers, 2. sour room, 3. salt room, 4. alkali room, 5. pole liquid chamber, 6. Bipolar Membrane, 7. anionic membrane, 8. cationic membrane, 9. Bipolar Membrane, 10. positive plate in figure, 11. negative plates, 12. power supplys; 13. feedstock circulation tanks, 14. pumps, 15. ultrapure waters, 16. pumps, 17. ultrapure waters, 18. pumps, 19. recycle pumps, 20. recycle pumps, 21. concentration are greater than 15% ~ 35%TBABr aqueous solution, 22. pumps, 23. discharge ports, 24. pumps, 25. discharge ports, 26. gas blowers, 27. venting ports, 28. gas blowers, 29. venting ports.
TBABr, Tetrabutyl amonium bromide; TBAOH, TBAH; TBA
+, TBuA ion; Br
-, bromide anion; OH
-, hydroxide radical; O
2, oxygen; Br
2, bromine; H
2, hydrogen.
Embodiment
The method of the high-purity TBAH of three compartment bipolar membrane electrodialysis device continuous production of the present invention adopts the reaction unit shown in accompanying drawing 1.
Prepare lower than 100 ppm bromide anions, high-purity TBAH time, the mass concentration in feedstock circulation tank 13 after treatment on ion exchange columns is 15% ~ 35% tetrabutyl phosphonium bromide aqueous ammonium, squeezes into salt room 3 through pump 14, controls raw material flow rate 500 ~ 2000 L/h; Positively charged ion TBA is produced in TBABr hydrolysis
+and negatively charged ion Br
-; Opening power 12, controls current density 300 ~ 1000 A/m
2, under infiltration with electric field action, positively charged ion TBA
+alkali room 4 is entered, negatively charged ion Br through cationic membrane 8
-sour room 2 is entered through anionic membrane; The TBABr do not permeated, through recycle pump 28, is greater than 15% ~ 30%TBABr aqueous solution 21 with mass concentration and mixes, and incoming stock circulation tank 13 reuses.
In alkali room 4, ultrapure water 17 is squeezed in alkali room 4 through pump 18, H
2o electrolysis generates positively charged ion H
+and negatively charged ion OH
-; Positively charged ion H
+pole liquid chamber 5 is entered through Bipolar Membrane 9 under electric field action; Negatively charged ion OH
-remain in alkali room 4, with the TBA entering alkali room 4 from salt room 3
+form TBAOH; Through pump 24 from discharge port 25 discharging.[note: during initial electrolysis, adds the TBAOH of 5-20%, to conduct electricity.】
In acid room 2, ultrapure water 15 is squeezed in sour room 2 through pump 16, and water electrolysis generates positively charged ion H
+and negatively charged ion OH
-; Negatively charged ion OH
-pole liquid chamber 1 is entered through Bipolar Membrane 6 under electric field action; Positively charged ion H
+remain in sour room 2, with the Br entering sour room 2 from salt room 3
-form HBr; Export from discharge port 23 through pump 22.[during initial electrolysis, add HBr, to conduct electricity.】
In pole liquid chamber 1, adding mass concentration is 3 ~ 5% aqueous sulfuric acids, recycles through recycle pump 19; The negatively charged ion OH of pole liquid chamber 1 is entered from sour room 2
-with Br
-, at a certain temperature, with positive plate effect, lose electronics and form O
2and Br
2, bring large quantity of air into through gas blower 26, by generated O
2with the micro-Br that infiltration is come
2discharge from venting port 27, harmful Br
2through alkali liquor absorption.
In pole liquid chamber 5, adding pole liquid mass concentration is 3 ~ 5% aqueous sulfuric acids, recycles through recycle pump 20; The positively charged ion H of pole liquid chamber 5 is entered from alkali room 4
+, with negative plate effect, obtain electronics and form H
2, the large quantity of air brought into gas blower 28, discharges from venting port 29.
Negatively charged ion Br in the TBAH exported by alkali room 4
-concentration is all less than 100 ppm, and product purity is higher.Current efficiency is 26 ~ 43%, and utilization rate of electrical is higher, save energy; Be convenient to adopt Automated condtrol, realize industrialization wide scale security and produce.
Below provide 3 embodiments of the present invention, each embodiment all adopts the device of Fig. 1.
embodiment 1
By 35% tetrabutyl phosphonium bromide aqueous ammonium, join in salt room 3, coutroi velocity is 2000h/L, connects direct current 12, controls each chambers temp 60 DEG C, controls constant current density at 600 A/m
2, obtain the TBAH aqueous solution that finished product content is 5%.Its bromide ion concentration is 33ppm; Current efficiency is 43%.
embodiment 2
By 35% tetrabutyl phosphonium bromide aqueous ammonium, join in salt room 3, coutroi velocity is 1000 h/L, connects direct current 12, controls each chambers temp 50 DEG C, controls constant current density at 600 A/m
2, obtain the TBAH aqueous solution that finished product content is 15%.Its bromide ion concentration is 29 ppm; Current efficiency is 39%.
embodiment 3
By 35% tetrabutyl phosphonium bromide aqueous ammonium, join in salt room 3, coutroi velocity is 1000 h/L, connects direct current 12, controls each chambers temp 30 DEG C, controls constant current density at 600 A/m
2, obtain the TBAH aqueous solution that finished product content is 15%.Its bromide ion concentration is 25 ppm; Current efficiency is 32%.
embodiment 4
By 15% tetrabutyl phosphonium bromide aqueous ammonium, join in salt room 3, coutroi velocity is 500 h/L, connects direct current 12, controls each chambers temp 60 DEG C, controls constant current density at 200A/m
2, obtain the TBAH aqueous solution that finished product content is 5%.Its bromide ion concentration is 31 ppm; Current efficiency is 31%.
embodiment 5
By 15% tetrabutyl phosphonium bromide aqueous ammonium, join in salt room 3, coutroi velocity is 2000 h/L, connects direct current 12, controls each chambers temp 30 DEG C, controls constant current density at 600 A/m
2, obtain the TBAH aqueous solution that finished product content is 20%.Its bromide ion concentration is 39 ppm; Current efficiency is 26%.
?comparative example's result shows, and the higher then current efficiency of temperature is higher, and concentration too high then current efficiency in alkali room declines; The too low then current efficiency of brine concentration declines.
Claims (9)
1. continuous electrolysis prepares a method for high-purity TBAH, it is characterized in that, adopt a kind of three compartment bipolar membrane electrodialysis devices, take Tetrabutyl amonium bromide as raw material, continuous production TBAH, adopts following implementation step:
(1) three compartment type bipolar membrane electrodialysis devices are formed with 1 Bipolar Membrane, 1 cationic exchange membrane and 1 anion-exchange membrane;
Three wherein said compartments are made up of electrodialysis compartment in the middle of two pole liquid chambers and;
Described intermediate chamber is made up of sour room, alkali room and salt room;
Described three compartment type bipolar membrane electrodialysis devices divide poling liquid chamber (1), sour room (2), salt room (3), alkali room (4), pole liquid chamber (5) successively; Bipolar Membrane (6) is accompanied between pole liquid chamber (1) and sour room (2); Anionic membrane (7) is accompanied between acid room (2) and salt room (3); Cationic membrane (8) is accompanied between salt room (3) and alkali room (4); Bipolar Membrane (9) is accompanied between alkali room (4) and pole liquid chamber (5); In pole liquid chamber (1), insert positive plate (10), in pole liquid chamber (5), insert negative plate (11);
(2) be tetrabutyl phosphonium bromide aqueous ammonium in feedstock circulation tank (13), squeeze into salt room (3) through pump (14), control raw material flow rate; Positively charged ion TBA is produced in TBABr hydrolysis
+and negatively charged ion Br
-; Opening power (12), controls current density, under osmosis and electric field action, and positively charged ion TBA
+alkali room (4) is entered, negatively charged ion Br through cationic membrane (8)
-sour room (2) is entered through anionic membrane; The TBABr do not permeated, through recycle pump (28), mixes with the TBABr aqueous solution (21), and incoming stock circulation tank (13) reuses;
(3) ultrapure water (17) is squeezed in alkali room (4) through pump (18), H
2o electrolysis generates positively charged ion H
+and negatively charged ion OH
-; Positively charged ion H
+pole liquid chamber (5) is entered through Bipolar Membrane (9) under electric field action; Negatively charged ion OH
-remain in alkali room (4), with the TBA entering alkali room (4) from salt room (3)
+form TBAOH; Through pump (24) from discharge port (25) discharging;
(4) ultrapure water (15) is squeezed in sour room (2) through pump (16), and water electrolysis generates positively charged ion H
+and negatively charged ion OH
-; Negatively charged ion OH
-pole liquid chamber (1) is entered through Bipolar Membrane (6) under electric field action; Positively charged ion H
+remain in sour room (2), with the Br entering sour room (2) from salt room (3)
-form HBr; Export from discharge port (23) through pump (22);
(5) the pole liquid in pole liquid chamber (1) recycles through recycle pump (19); The negatively charged ion OH of pole liquid chamber (1) is entered from sour room (2)
-with Br
-, at a certain temperature, with positive plate effect, lose electronics and form O
2and Br
2, bring large quantity of air into, by generated O through gas blower (26)
2with the micro-Br that infiltration is come
2discharge, through alkali liquor absorption from venting port (27);
(6) the pole liquid in pole liquid chamber (5) recycles through recycle pump (20); The positively charged ion H of pole liquid chamber (5) is entered from alkali room (4)
+, with negative plate effect, obtain electronics and form H
2, the large quantity of air brought into gas blower (28), discharges from venting port (29).
2. a kind of continuous electrolysis according to claim 1 prepares the method for high-purity TBAH, it is characterized in that, be mass concentration 15% ~ 35% tetrabutyl phosphonium bromide aqueous ammonium in head tank (13) described in step (2), need, through treatment on ion exchange columns, to obtain high-purity raw.
3. a kind of continuous electrolysis according to claim 1 prepares the method for high-purity TBAH, it is characterized in that, the mass concentration of the TBABr aqueous solution (21) described in step (2) is greater than 15% ~ 35%.
4. a kind of continuous electrolysis according to claim 1 prepares the method for high-purity TBAH, it is characterized in that, controlling raw material flow rate described in step (2) is 500 ~ 2000 L/h.
5. a kind of continuous electrolysis according to claim 1 prepares the method for high-purity TBAH, it is characterized in that, the current density controlling bipolar membrane electrodialysis device described in step (2) is 200 ~ 600 A/m
2.
6. a kind of continuous electrolysis according to claim 1 prepares the method for high-purity TBAH, it is characterized in that, described in the pole liquid in pole liquid chamber 1 described in step (4) and step (5), the pole liquid of pole liquid chamber (5) is mass concentration is 3 ~ 5% aqueous sulfuric acids.
7. a kind of continuous electrolysis according to claim 1 prepares the method for high-purity TBAH, it is characterized in that, controlling temperature of reaction in preparation process is 30 ~ 60 DEG C.
8. a kind of continuous electrolysis according to claim 1 prepares the method for high-purity TBAH, it is characterized in that, the high-purity TBAH mass concentration obtained is 5% ~ 20% aqueous solution.
9. a kind of continuous electrolysis according to claim 1 prepares the method for high-purity TBAH, it is characterized in that, in the high-purity TPAOH prepared, bromide ion concentration is less than 100 ppm.
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| CN105294455A (en) * | 2015-10-09 | 2016-02-03 | 南京工业大学 | Method for preparing aqueous tetrabutylammonium hydroxide solvent by anion exchange |
| CN106801233A (en) * | 2017-01-11 | 2017-06-06 | 浙江工业大学 | A kind of electrolysis prepares the system and method for high-purity TPAOH |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6207039B1 (en) * | 1998-04-07 | 2001-03-27 | Sachem, Inc. | Process for recovering onium hydroxides or onium salts from solutions containing onium compounds using electrochemical ion exchange |
| US20030155244A1 (en) * | 2000-04-19 | 2003-08-21 | Ellenio Mischi | Method for making a bipolar membrane and use of resulting bipolar membrane |
| CN101597763A (en) * | 2009-06-09 | 2009-12-09 | 建德市新德化工有限公司 | A kind of preparation method of efficient tetramethylammonium hydroxide |
| CN102510853A (en) * | 2009-09-24 | 2012-06-20 | 株式会社德山 | Process for production of tetraalkylammonium hydroxide |
| CN102531927A (en) * | 2011-12-28 | 2012-07-04 | 浙江工业大学 | Method for preparing tetrapropyl ammonium hydroxide by utilizing bipolar membrane electrodialysis |
| CN103073131A (en) * | 2012-12-28 | 2013-05-01 | 中国环境科学研究院 | Process for treating amantadine bromination waste water and mineral acid and alkali recycling through bipolar membrane electrodialysis process |
| CN103922980A (en) * | 2014-04-22 | 2014-07-16 | 中国科学技术大学 | Method for separating methionine from mixed solution of methionine salt and carbonate by using bipolar membrane electrodialysis |
-
2014
- 2014-09-30 CN CN201410516813.6A patent/CN104278288A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6207039B1 (en) * | 1998-04-07 | 2001-03-27 | Sachem, Inc. | Process for recovering onium hydroxides or onium salts from solutions containing onium compounds using electrochemical ion exchange |
| US20030155244A1 (en) * | 2000-04-19 | 2003-08-21 | Ellenio Mischi | Method for making a bipolar membrane and use of resulting bipolar membrane |
| CN101597763A (en) * | 2009-06-09 | 2009-12-09 | 建德市新德化工有限公司 | A kind of preparation method of efficient tetramethylammonium hydroxide |
| CN102510853A (en) * | 2009-09-24 | 2012-06-20 | 株式会社德山 | Process for production of tetraalkylammonium hydroxide |
| CN102531927A (en) * | 2011-12-28 | 2012-07-04 | 浙江工业大学 | Method for preparing tetrapropyl ammonium hydroxide by utilizing bipolar membrane electrodialysis |
| CN103073131A (en) * | 2012-12-28 | 2013-05-01 | 中国环境科学研究院 | Process for treating amantadine bromination waste water and mineral acid and alkali recycling through bipolar membrane electrodialysis process |
| CN103922980A (en) * | 2014-04-22 | 2014-07-16 | 中国科学技术大学 | Method for separating methionine from mixed solution of methionine salt and carbonate by using bipolar membrane electrodialysis |
Cited By (15)
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|---|---|---|---|---|
| CN105112934A (en) * | 2015-09-16 | 2015-12-02 | 青岛润兴光电材料有限公司 | Preparation method for tetra-alkyl ammonium hydroxide |
| CN105294455A (en) * | 2015-10-09 | 2016-02-03 | 南京工业大学 | Method for preparing aqueous tetrabutylammonium hydroxide solvent by anion exchange |
| CN106801233A (en) * | 2017-01-11 | 2017-06-06 | 浙江工业大学 | A kind of electrolysis prepares the system and method for high-purity TPAOH |
| CN106801233B (en) * | 2017-01-11 | 2019-02-01 | 浙江工业大学 | A kind of electrolysis method prepares the system and method for high-purity tetrapropylammonium hydroxide |
| CN108467347A (en) * | 2018-03-22 | 2018-08-31 | 新乡化纤股份有限公司 | A method of electrolysis tetrabutyl ammonium sulfate recycles tetrabutylammonium hydroxide |
| CN108486604A (en) * | 2018-03-26 | 2018-09-04 | 新乡化纤股份有限公司 | A method of preparing tetrabutylammonium hydroxide by raw material of tetrabutyl ammonium sulfate |
| CN109134266A (en) * | 2018-09-21 | 2019-01-04 | 南京元亨化工科技有限公司 | A method of based on the high-purity tetrapropylammonium hydroxide of composite bipolar film electrolytic preparation |
| CN109265358A (en) * | 2018-09-21 | 2019-01-25 | 南京元亨化工科技有限公司 | A method of based on electron ion exchange system for high-purity tetrapropylammonium hydroxide |
| CN109134266B (en) * | 2018-09-21 | 2021-06-15 | 南京元亨化工科技有限公司 | Method for preparing high-purity tetrapropyl ammonium hydroxide based on composite bipolar membrane electrolysis |
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| CN110079822A (en) * | 2019-05-31 | 2019-08-02 | 中触媒新材料股份有限公司 | A kind of system and method that three films, four Room electrolysis method prepares tetra-alkyl ammonium hydroxide |
| CN110158114A (en) * | 2019-05-31 | 2019-08-23 | 中触媒新材料股份有限公司 | A kind of three films, the four Room electrolysis system preparing tetra-alkyl ammonium hydroxide and method |
| CN110318066A (en) * | 2019-06-20 | 2019-10-11 | 青岛鼎海电化学科技有限公司 | A kind of preparation method of tetra-alkyl ammonium hydroxide |
| CN110644014A (en) * | 2019-10-30 | 2020-01-03 | 盐城泛安化学有限公司 | Preparation method of tetraethyl ammonium hydroxide |
| CN113265683A (en) * | 2021-05-12 | 2021-08-17 | 肯特催化材料股份有限公司 | High-efficiency production process of tetrapropylammonium hydroxide and tetrapropylammonium hydroxide aqueous solution prepared by high-efficiency production process |
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