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Green preparation method of tetramethylammonium hydroxide

A technology of tetramethylammonium hydroxide and ruthenium dioxide-titanium substrate, which is applied in the field of electrolytic chemistry and electrochemistry, and can solve problems such as complex equipment, short process flow, and reduced energy efficiency

Active Publication Date: 2020-11-20
信联电子材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Chinese patent application CN103388155A discloses a device and method for continuously preparing tetramethylammonium hydroxide, the purpose of which is to solve the problems of high production cost and high impurity content in existing tetramethylammonium hydroxide production methods. The device includes Ion exchange column, electrolytic cell, anode raw material tank, cathode raw material tank, cathode gas storage tank, anode gas storage tank, boiler, heating tank, first liquid pump, second liquid pump, third liquid pump, first pipeline, second 2nd pipeline, 3rd pipeline, 4th pipeline
The process is short, the operation is simple, and the production cost is low. At the same time, the prepared product has high purity and high yield, which effectively reduces energy efficiency, overcomes the shortcomings of high power consumption and low current efficiency in the prior art, and can adapt to industrial production. needs
[0014] However, the equipment of the above-mentioned patent application is relatively complicated and has high requirements on raw materials; it is difficult to obtain high current efficiency and product purity at the same time

Method used

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  • Green preparation method of tetramethylammonium hydroxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1-Preparation of polystyrene nanospheres

[0046] Weigh out 0.080g SDS and 0.15g sodium bicarbonate and add 300mL deionized water. The mixture was stirred evenly and the temperature was raised to 80°C. Add 35mL styrene monomer and react for 2h; then add 0.15g potassium persulfate, and react at a constant temperature for 12h at a stirring speed of 200rpm. After the reaction is over, stop heating and cool naturally. Anhydrous ethanol was added to the polymerization solution, centrifuged three times repeatedly, and dried in vacuum to obtain polystyrene nanospheres with an average particle size of 122 nm. Before use, the polystyrene nanospheres were prepared into an 8wt% solution using absolute ethanol, and ultrasonically dispersed into a uniform polystyrene nanosphere suspension.

Embodiment 2

[0047] Example 2-Preparation of TiO 2 Nanosphere sol

[0048] Add 25 mL of isopropyl titanate to 80 mL of absolute ethanol, stir evenly, and add 10 mL of diethanolamine dropwise. Then 50 mL of anhydrous ethanol deionized water solution with a volume ratio of 5:1 was slowly added dropwise thereto. After the addition is complete, continue to stir for 6h to obtain TiO with an average particle size of 54nm 2 Nanosphere sol.

Embodiment 3

[0049] Example 3-Electrolytic preparation of anode for tetramethylammonium hydroxide

[0050] The titanium substrate was heated at 50° C. for 90 min through a 0.3M oxalic acid solution to obtain a titanium substrate with the oxide layer removed. The titanium substrate with the oxide layer removed was immersed in the polystyrene nanosphere suspension of Example 1, and a layer of polystyrene nanosphere film was plated by the pulling method at a pulling rate of 1 mm / s, and then dried naturally; It is immersed in the TiO of Example 2 2 In the nanosphere sol, a layer of TiO is plated by the pulling method 2 The nanosphere sol film has a pulling rate of 1 mm / s; a titanium substrate plated with a single-layer composite film is obtained. The titanium substrate coated with the single-layer composite film is fully dried; the drying condition is drying at 80° C. for 30 min. Repeat the above steps (1) and (2) to obtain a titanium substrate coated with a multilayer composite film until the t...

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Abstract

The invention discloses a green preparation method of tetramethylammonium hydroxide. According to the method, a double-chamber single-membrane electrolytic cell is adopted, a ruthenium dioxide titanium substrate is taken as an anode of the electrolytic cell, stainless steel is taken as a cathode of the electrolytic cell, a cell body is made of a polytetrafluoroethylene material, and a perfluorocartankylic acid / sulfonic acid composite ionic membrane is taken as a cation exchange membrane of the electrolytic cell; and constant-current electrolysis on the electrolyte in the electrolytic cell is carried out. The method has relatively high current efficiency and relatively high product purity, and can fully meet the requirements of cleaning and corrosion in the field of electronic industry.

Description

Technical field [0001] The invention belongs to the technical field of electrochemistry, especially the technical field of electrolysis chemistry; it relates to a green preparation method of tetramethylammonium hydroxide. Background technique [0002] Tetramethylammonium hydroxide, also known as tetramethylammonium hydroxide, has the structural formula (CH 3 ) 4 NOH, whose English name is tetramethylammonium hydroxide (TMAH for short), is one of the strongest organic bases, and its basicity is similar to the inorganic bases NaOH and KOH. [0003] As a tetramethylammonium hydroxide product on the market, it is mainly divided into two categories: industrial grade and electronic grade. Electronic grade tetramethylammonium hydroxide is a colorless and transparent mixed liquid of tetramethylammonium hydroxide and water. Typically, tetramethylammonium hydroxide is formulated into 10% (wt%) and 25% (wt%) aqueous solutions. As measured by Toyo Chemical Co., Ltd., the specific gravity of ...

Claims

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Application Information

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IPC IPC(8): C25B3/00C25B9/08C25B11/06
CPCC25B3/00
Inventor 刘颂军孙炜孟鹏
Owner 信联电子材料科技股份有限公司
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