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CN102400173B - Method for preparing electronic grade tetramethylammonium hydroxide by continuous method - Google Patents

Method for preparing electronic grade tetramethylammonium hydroxide by continuous method Download PDF

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CN102400173B
CN102400173B CN201110380374.7A CN201110380374A CN102400173B CN 102400173 B CN102400173 B CN 102400173B CN 201110380374 A CN201110380374 A CN 201110380374A CN 102400173 B CN102400173 B CN 102400173B
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tetramethylammonium hydroxide
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赵文洲
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Zhenjiang Runjing High Purity Chemical Technology Co., Ltd
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Abstract

The invention discloses a method for preparing electronic grade tetramethylammonium hydroxide by a continuous method. The method comprises the following steps of: sequentially dividing an electrolytic cell into a cathode chamber, a first cathode middle chamber, a second cathode middle chamber and an anode chamber, wherein the two adjacent chambers are partitioned by a cation exchange membrane and connected by using a circulating pump and a filter connected in series, and the anode chamber is connected with the circulating pump and the filter connected in series; putting a 5 to 50 percent aqueous solution of a tetramethyl ammonium salt into the anode chamber, wherein (CH3)4N<+>, H<+> and metal cation R<+> in the solution enter the two cathode middle chambers and the cathode chamber through the cation exchange membranes; and removing the sediment generated by partial metal cation R<+> and OH<-> by using the filter, pumping the filtrate for reaction by using the circulating pump, and discharging the 5 to 30 percent tetramethylammonium hydroxide from the cathode chamber, wherein the concentration of each metal ion is less than 10ppb, the concentration of each anion is less than 500ppb, and the tetramethylammonium hydroxide has high purity. The current efficiency of the tetramethylammonium hydroxide is 70 to 80 percent, the tetramethylammonium hydroxide has high utilization rate, and the method has no pollution and can be used for large-scale production.

Description

The method of preparing electronic grade tetramethylammonium hydroxide by continuous method
Technical field
The present invention relates to a kind of preparation method of Tetramethylammonium hydroxide, refer in particular to and take tetramethyl ammonium as raw material, by continous way electrolytic process, prepare the method for electronic-grade Tetramethylammonium hydroxide.
Background technology
Tetramethylammonium hydroxide (TMAH) is important industry and electronic chemical product, has been widely used, as the catalyzer synthesizing for organosilicon series product, for fields such as polyester polymerization, weaving, plastics and leathers at industrial circle.Electronic-grade Tetramethylammonium hydroxide is mainly used on liquid crystal panel and chip as developing solution.
At present, production Tetramethylammonium hydroxide all adopts oxidation patina method, by tetramethyl ammonium chloride, is reacted generation Tetramethylammonium hydroxide with silver suboxide, and the defect of the operational path of the method is: 1, can only batch production, and cannot scale production; 2, need to consume valuable silver suboxide, cost is higher; 3, in the Tetramethylammonium hydroxide generating, contain micro-silver ions, make Tetramethylammonium hydroxide be subject to the pollution of silver ions.The purity of the Tetramethylammonium hydroxide 4, generating is lower, and wherein each concentration of metal ions is big or small 50 ppb all, and each anion concentration is all greater than 550 ppb.
Summary of the invention
A kind of method that the object of the invention is to provide for overcoming the deficiency of existing oxidation patina method production Tetramethylammonium hydroxide preparing electronic grade tetramethylammonium hydroxide by continuous method, cost is low, pollution-free, and prepared electronic-grade Tetramethylammonium hydroxide purity is high.
The technical solution used in the present invention is employing following steps: A, an electrolyzer is divided into cathode compartment, the first negative electrode intermediate chamber, the second negative electrode intermediate chamber and anolyte compartment successively, between every two adjacent chambers, with cationic exchange membrane, is separated by; In cathode compartment and anolyte compartment, insert respectively cathode plate and plate, with the recycle pump of serial connection, with strainer, two adjacent Room are connected respectively to recycle pump and the strainer that ,Qie anolyte compartment self is connected serial connection respectively; Electric current between B, connection cathode plate and plate, the tetramethyl-ammonium salt brine solution that is 5%~50% by material concentration is put into anolyte compartment, and tetramethyl-ammonium salt hydrolysis generates positively charged ion (CH 3) 4n +and negatively charged ion X -, (CH 3) 4n +, H +, the metallic cation R in solution +seeing through cationic exchange membrane enters in the second negative electrode intermediate chamber, the first negative electrode intermediate chamber and cathode compartment; Negatively charged ion X -with OH -after arriving plate, produce gas discharge, part metals positively charged ion R +with OH -generate throw out, throw out and rest part metallic cation are removed by strainer when recycle pump internal recycle; C, in the second negative electrode intermediate chamber, the first negative electrode intermediate chamber and cathode compartment, positively charged ion (CH 3) 4n +with OH -production Tetramethylammonium hydroxide (CH 3) 4nOH, part metals positively charged ion R +with OH -the throw out generating is removed by strainer after recycle pump, and filtrate is recycled in pump blowback anolyte compartment, the second negative electrode intermediate chamber and the first negative electrode intermediate chamber to be reacted; D, the Tetramethylammonium hydroxide output that is 5%~30% by concentration in cathode compartment.
The invention has the advantages that: adopt four Room three film ionic membrane continous way electrolytic process to prepare electronic-grade Tetramethylammonium hydroxide, the drawback that to have solved technique be in the past only batch production, be difficult to scale operation, product purity is high, can meet the need of production of most advanced and sophisticated high-tech area.In addition, also comparatively safe, green with electrolytic process production, can effectively reduce the generation of three industrial wastes, pollution-free, and utilization rate of electrical is high.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Fig. 1 is the electrolysis reaction device of four Room three film ionic membranes of the present invention and the medium schematic diagram in chamber;
1. cathode compartment; 2. the first negative electrode intermediate chamber; 3. the second negative electrode intermediate chamber; 4. anolyte compartment; 5. strainer; 6. rectifier; 7. alternating-current; 8. cathode plate; 9. plate; 10. opening for feed; 11. discharge ports; 12. cationic exchange membranes; 13. recycle pumps;
R 1 +for tetramethylammonium cation; R +for metallic cation; X -for various negatively charged ion; Gas is the gases such as oxygen, chlorine, carbonic acid gas.
Embodiment
The method of preparing electronic grade tetramethylammonium hydroxide by continuous method of the present invention adopts the electrolysis reaction device shown in accompanying drawing 1, this electrolysis reaction device has an electrolyzer, three cationic exchange membranes 12 are divided into four chambers by electrolyzer, electrolyzer is comprised of continuously arranged four Room, cathode compartment 1, the first negative electrode intermediate chamber 2, the second negative electrode intermediate chamber 3 and anolyte compartment 4 from left to right successively, Ji Yige anolyte compartment, three cathode compartments.Between every two adjacent chambers, with cationic exchange membrane 12, separate, be between cathode compartment 1 and the first negative electrode intermediate chamber 2, between the first negative electrode intermediate chamber 2 and the second negative electrode intermediate chamber 3, all use cationic exchange membrane 12 to separate between the second negative electrode intermediate chamber 3 and anolyte compartment 4, cationic exchange membrane 12 is cation exchange resin membranes.
In cathode compartment 1, insert cathode plate 8, the material of cathode plate 8 is nickel or graphite; In anolyte compartment 4, insert plate 9, the material of plate 9 is titanium, and cathode plate 8 and plate 9 all adopt oxide covering, and the material of oxide covering is analysed chlorine coating for analysing oxygen.Between cathode plate 8 and plate 9, be connected in series rectifier 6, rectifier 6 incoming transport electricity 7.
Utilize recycle pump 13 and strainer 5 that each adjacent utmost point chamber is connected, make the electrolysis liquid phase circulation in adjacent chamber, the two poles of the earth, with the highly purified Tetramethylammonium hydroxide of continuous production.Specifically between cathode compartment 1 and the first negative electrode intermediate chamber 2, connect the recycle pump 13 and strainer 5 of serial connection mutually, the electrolytic solution of cathode compartment 1 output enters the first negative electrode intermediate chamber 2 through filter 5 again after recycle pump 13.Between the first negative electrode intermediate chamber 2 and the second negative electrode intermediate chamber 3, the same recycle pump 13 of serial connection mutually that connects enters the second negative electrode intermediate chamber 3 through filter 5 with the electrolytic solution of strainer 5, the first negative electrode intermediate chamber 2 outputs again after recycle pump 13.Between the second negative electrode intermediate chamber 3 and anolyte compartment 4, also connect the recycle pump 13 of serial connection mutually and after recycle pump 13, through filter 5, enter anolyte compartment 4 with the electrolytic solution of strainer 5, the second negative electrode intermediate chamber 3 outputs again.Anolyte compartment 4 self connects the recycle pump 13 and strainer 5 of serial connection mutually, realizes the internal recycling of anolyte compartment 4.
While preparing electronic-grade Tetramethylammonium hydroxide, the tetramethyl-ammonium salt brine solution that is first 5%~50% by material concentration is put into anolyte compartment 4 from opening for feed 10, and tetramethyl ammonium is wherein a kind of in tetramethyl ammonium hydrogen carbonate, tetramethyl-carboxylic acid ammonium, tetramethyl-ammonium formiate, tetramethyl ammonium acetate, tetramethyl-ammonium halide, tetramethyl-ammonium sulfate or tetramethyl-ammonium nitrate.Plate 9 in incoming transport electricity 7 ,Shi anolyte compartments 4 and cathode plate 8 making current in cathode compartment 1, making current density is 1000~2000 A/m 2.In anolyte compartment 4, tetramethyl-ammonium salt hydrolysis generates (CH 3) 4n +and negatively charged ion X -, water can be hydrolyzed and generate H +and OH -.Positively charged ion (CH 3) 4n +, H +with the metallic cation R in solution +see through cationic exchange membrane 12 and enter the second negative electrode intermediate chamber 3.And negatively charged ion X -with OH -arrive plate 9, lose the gas gas such as electron production oxygen and chlorine, carbonic acid gas, these gases are discharged from pore.Part metals positively charged ion R +as Ca +, Mg +deng meeting and OH -generate throw out.Throw out and rest part metallic cation Na +with K +during the internal recycle of Deng anolyte compartment 4 self, by strainer 5, removed.
In the second negative electrode intermediate chamber 3, positively charged ion (CH 3) 4n +oH with water hydrolysis generation -production Tetramethylammonium hydroxide (CH 3) 4nOH, part metals positively charged ion R +with OH -generate throw out.By the recycle pump 13 of contacting mutually, with strainer 5, the second negative electrode intermediate chamber 3 is connected to throw out and rest part metallic cation Na with anolyte compartment 4 +with K +deng through filter 5, remove, filtrate is continued reaction in 4 , anolyte compartments 4, recycle pump 13 blowback anolyte compartment.The Tetramethylammonium hydroxide concentration obtaining is 1%~20%.
In the first negative electrode intermediate chamber 2, positively charged ion (CH 3) 4n +oH with water hydrolysis generation -production Tetramethylammonium hydroxide (CH 3) 4nOH, part metals positively charged ion R +with OH -generate throw out.By the recycle pump 13 of contacting mutually, with strainer 5, the first negative electrode intermediate chamber 2 is connected to throw out and part metals positively charged ion R with the second negative electrode intermediate chamber 3 +through filter 13, remove, filtrate continuation is recycled pump 13 and is pumped back to reaction in the second negative electrode intermediate chamber 3.Obtain concentration and be 3%~25% Tetramethylammonium hydroxide.
In cathode compartment 1, positively charged ion (CH 3) 4n +oH with water hydrolysis generation -production Tetramethylammonium hydroxide (CH 3) 4nOH, H +arrive cathode plate 8 and obtain the oxidized generation of electronics H 2.Meanwhile, through recycle pump 13, with strainer 5, cathode compartment 1 is connected to part metals positively charged ion R with the first negative electrode intermediate chamber 2 +with OH -generate throw out and removed by strainer 5 by recycle pump 13, filtrate continuation is recycled pump 13 and is pumped back to reaction in the first negative electrode intermediate chamber 2.The Tetramethylammonium hydroxide that is 5%~30% by the concentration obtaining in cathode compartment 1 is from discharge port 11 outputs of cathode compartment 1 bottom.
The present invention, through selection and the multiple stage circulation of multistage cationic membrane, can obtain the Tetramethylammonium hydroxide of electronic-grade purity.In the process of reaction, because water is raw material, simultaneously also need to be in anolyte compartment 4 make up water.Each concentration of metal ions in the Tetramethylammonium hydroxide of being exported by cathode compartment 1 is all less than 10 ppb, and each anion concentration is all less than 500 ppb, and purity is higher.Current efficiency is 70 ~ 90%, and utilization rate of electrical is high, save energy, and cost is also low.
5 embodiment of the present invention are below provided, and each embodiment all adopts the device of Fig. 1.
embodiment 1
Plate 9 electrode materialss are titanium, and cathode plate 8 electrode materialss are nickel, and pole plate employing is analysed oxygen and analysed chlorine coating, adopts the current density of 1000 A/ ㎡.Electrolytic solution in cathode compartment 1, the first negative electrode intermediate chamber 2, the second negative electrode intermediate chamber 3, anolyte compartment 4 in adjacent two Room all carries out outer circulation with recycle pump 13 each other, and anolyte compartment 4 self carries out internal recycle with recycle pump 13.In anolyte compartment 4, be that concentration is the salts solution of 50% tetramethyl ammonium hydrogen carbonate, in the second negative electrode intermediate chamber 3, be that concentration is 20% Tetramethylammonium hydroxide, in the first negative electrode intermediate chamber 2, be that concentration is 3% Tetramethylammonium hydroxide, in cathode compartment 1, be that concentration is 30% Tetramethylammonium hydroxide, current efficiency is 70%.
Connect the electric current between two-plate, can prepare electronic-grade Tetramethylammonium hydroxide by continuous electrolysis, each concentration of metal ions in the electronic-grade Tetramethylammonium hydroxide of preparation is all less than 10 ppb, and carbonate is less than 500 ppb(in Table 1).
embodiment 2
Plate 9 electrode materialss are titanium, and cathode plate 8 electrode materialss are graphite, and pole plate employing is analysed oxygen and analysed chlorine coating, adopts the current density of 1500 A/ ㎡.The pump Recycle design of the electrolytic solution in each chamber is identical with embodiment 1.In anolyte compartment 4, be that concentration is 40% tetramethyl ammonium hydrogen carbonate solution, in the second negative electrode intermediate chamber 3, be that concentration is 10% Tetramethylammonium hydroxide, in the first negative electrode intermediate chamber 2, be that concentration is 10% Tetramethylammonium hydroxide, in cathode compartment 1, be that concentration is 15% Tetramethylammonium hydroxide, current efficiency is 90%.
Connect the electric current between two-plate, can prepare electronic-grade Tetramethylammonium hydroxide by continuous electrolysis, in the electronic-grade Tetramethylammonium hydroxide of preparation, each concentration of metal ions is less than 10 ppb, and carbonate is less than 500 ppb(in Table 1).
embodiment 3
Plate 9 electrode materialss are titanium, and cathode plate 8 electrode materialss are graphite, and pole plate employing is analysed oxygen and analysed chlorine coating, adopts the current density of 2000 A/ ㎡.The pump Recycle design of the electrolytic solution in each chamber is identical with embodiment 1.In anolyte compartment 4, be that concentration is 5% tetramethyl ammonium hydrogen carbonate solution, in the second negative electrode intermediate chamber 3, be that concentration is 1% Tetramethylammonium hydroxide, in the first negative electrode intermediate chamber 2, be that concentration is 4% Tetramethylammonium hydroxide, in cathode compartment 1, be that concentration is 5% Tetramethylammonium hydroxide, current efficiency is 83%.
Connect the electric current between two-plate, can prepare electronic-grade Tetramethylammonium hydroxide by continuous electrolysis, in the electronic-grade Tetramethylammonium hydroxide of preparation, each concentration of metal ions is all less than 10 ppb (in Table 1), and carbonate is less than 500 ppb.
embodiment 4
Plate 9 electrode materialss are titanium, and cathode plate 8 electrode materialss are graphite, and pole plate employing is analysed oxygen and analysed chlorine coating, adopts the current density of 1700A/ ㎡.The pump Recycle design of the electrolytic solution in each chamber is identical with embodiment 1.In anolyte compartment 4, be that concentration is 10% tetramethyl ammonium hydrogen carbonate solution, in the second negative electrode intermediate chamber 3, be that concentration is 15% Tetramethylammonium hydroxide, in the first negative electrode intermediate chamber 2, be that concentration is 20% Tetramethylammonium hydroxide, in cathode compartment 1, be that concentration is 30% Tetramethylammonium hydroxide, current efficiency is 90%.
Connect the electric current between two-plate, can prepare electronic-grade Tetramethylammonium hydroxide by continuous electrolysis, in the electronic-grade Tetramethylammonium hydroxide of preparation, each concentration of metal ions is all less than 10 ppb, and carbonate is less than 500 ppb(in Table 1).
Metal ion and carbonate content in the Tetramethylammonium hydroxide of table 1 preparation
Figure 831829DEST_PATH_IMAGE002
embodiment 5
With embodiment 2, tetramethyl ammonium hydrogen carbonate in difference Shi Jinjiang anolyte compartment 4 changes tetramethyl-carboxylic acid ammonium, tetramethyl-ammonium formiate, tetramethyl ammonium acetate, tetramethyl-ammonium halide, tetramethyl-ammonium sulfate and tetramethyl-ammonium nitrate into, each concentration of metal ions in prepared electronic-grade Tetramethylammonium hydroxide is all less than 10 ppb, and each anion concentration is all less than 500 ppb(in Table 2); Current efficiency is 83%.
Anion concentration in product when the different tetramethyl ammoniums of table 2 are raw material

Claims (4)

1. a method for preparing electronic grade tetramethylammonium hydroxide by continuous method, is characterized in that adopting following steps:
A, an electrolyzer is divided into cathode compartment (1), the first negative electrode intermediate chamber (2), the second negative electrode intermediate chamber (3) and anolyte compartment (4) successively, between every two adjacent chambers, with cationic exchange membrane (12), is separated by; In cathode compartment (1) and anolyte compartment (4), insert respectively cathode plate (8) and plate (9), with the recycle pump (13) of serial connection, with strainer (5), two adjacent Room are connected respectively to the recycle pump (13) and strainer (5) that ,Qie anolyte compartment (4) self is connected serial connection respectively;
Electric current between B, connection cathode plate (8) and plate (9), the tetramethyl-ammonium salt brine solution that is 5%~50% by material concentration is put into anolyte compartment (4), and tetramethyl-ammonium salt hydrolysis generates positively charged ion (CH 3) 4n +and negatively charged ion X -, (CH 3) 4n +, H +, the metallic cation R in solution +seeing through cationic exchange membrane (12) enters in the second negative electrode intermediate chamber (3), the first negative electrode intermediate chamber (2) and cathode compartment (1); Negatively charged ion X -with OH -after arriving plate (9), produce gas discharge, part metals positively charged ion R +with OH -generate throw out, throw out and rest part metallic cation are removed by strainer (5) when recycle pump (13) internal recycle;
C, in the second negative electrode intermediate chamber (3), the first negative electrode intermediate chamber (2) and cathode compartment (1), positively charged ion (CH 3) 4n +with OH -production Tetramethylammonium hydroxide (CH 3) 4nOH, part metals positively charged ion R +with OH -the throw out generating is removed by strainer (5) after recycle pump (13), and filtrate is recycled reaction in pump (13) blowback anolyte compartment (4), the second negative electrode intermediate chamber (3) and the first negative electrode intermediate chamber (2);
D, the Tetramethylammonium hydroxide output that is 5%~30% by concentration in cathode compartment (1).
2. the method for preparing electronic grade tetramethylammonium hydroxide by continuous method according to claim 1, is characterized in that: described tetramethyl ammonium is tetramethyl ammonium hydrogen carbonate, tetramethyl-carboxylic acid ammonium, tetramethyl-ammonium formiate, tetramethyl ammonium acetate, tetramethyl-ammonium halide, tetramethyl-ammonium sulfate or tetramethyl-ammonium nitrate.
3. the method for preparing electronic grade tetramethylammonium hydroxide by continuous method according to claim 1, it is characterized in that: the Tetramethylammonium hydroxide concentration in the first negative electrode intermediate chamber (2) is that the Tetramethylammonium hydroxide concentration in the 3%~25%, second negative electrode intermediate chamber (3) is 1%~20%.
4. the method for preparing electronic grade tetramethylammonium hydroxide by continuous method according to claim 1, it is characterized in that: cathode plate (8) material is nickel or graphite, plate (9) material is titanium, and cathode plate (8) and plate (9) all adopt analyses oxygen and analyse oxychlorination coating.
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CN103388155B (en) * 2013-07-31 2015-07-08 自贡天龙化工有限公司 Device and method for continuously preparing tetramethylammonium hydroxide
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CN104630818B (en) * 2015-02-13 2017-07-21 赵文洲 The method that the film continuous electrolysis of three Room two prepares high-purity benzyltrimethylammonium hydroxide
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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
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CN1523135A (en) * 2003-02-18 2004-08-25 �Ͼ���ҵ��ѧ Process for preparing tetramethyl ammonium hydroxide by electrolysis-electrodialysis
DE10317029A1 (en) * 2003-04-11 2004-10-21 Basf Ag Preparation of quaternary ammonium hydroxides, useful in photoresist developers for microelectronics, by electrolysis of the corresponding salt in a divided cell that has an intermediate chamber of ion exchanger
CN102206832A (en) * 2011-04-29 2011-10-05 郑州大学 Method for preparing electronic-grade tetramethylammonium hydroxide (TMAH)

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