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Preparation method of electronic-grade tetramethylammonium hydroxide

A technology of tetramethylammonium hydroxide and ruthenium dioxide titanium substrate is applied in the fields of electrochemistry and electrolysis chemistry, and can solve the problems of low production cost, low current efficiency and high yield

Active Publication Date: 2020-11-20
CANGZHOU SUNHEAT CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Preparation method of electronic-grade tetramethylammonium hydroxide
  • Preparation method of electronic-grade tetramethylammonium hydroxide

Examples

Experimental program
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Effect test

Embodiment 1

[0048] Embodiment 1—preparation of polystyrene nanospheres

[0049] Weigh 0.080g SDS and 0.15g sodium bicarbonate, add to 300mL deionized water. The mixture was stirred evenly, and the temperature was raised to 80°C. Add 35 mL of styrene monomer and react for 2 hours; then add 0.15 g of potassium persulfate and react at constant temperature for 12 hours at a stirring speed of 200 rpm. After the reaction was over, the heating was stopped and allowed to cool naturally. Add absolute ethanol to the polymerization solution, centrifuge repeatedly 3 times, and vacuum dry to obtain polystyrene nanospheres with an average particle diameter of 122 nm. Before use, the polystyrene nanospheres were prepared into an 8wt% solution using absolute ethanol, and ultrasonically dispersed into a uniform suspension of polystyrene nanospheres.

Embodiment 2

[0050] Embodiment 2—Preparation of TiO 2 nanosphere sol

[0051] Add 25 mL of isopropyl titanate into 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 dropwise addition, continue to stir for 6h to obtain TiO with an average particle size of 54nm. 2 nanosphere sol.

Embodiment 3

[0052] Embodiment 3—electrolytically prepares the anode of tetramethylammonium hydroxide

[0053] The titanium substrate was heated at 50° C. for 90 minutes through a 0.3 M oxalic acid solution to obtain a titanium substrate from which the oxide layer was removed. Immerse the titanium substrate from which the oxide layer was removed in the polystyrene nanosphere suspension of Example 1, and plate a layer of polystyrene nanosphere film by the pulling method, with a pulling rate of 1mm / s, and then dry naturally; It is immersed in the TiO of Example 2 2 In the nanosphere sol, a layer of TiO was plated by the pulling method 2 The nanosphere sol film was pulled at a rate of 1 mm / s; a titanium substrate coated with a single-layer composite film was obtained. Fully dry the titanium substrate coated with a single-layer composite film; the drying condition is to dry at 80° C. for 30 minutes. Repeat the above steps (1) and (2) to obtain a titanium substrate coated with a multilayer c...

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Abstract

The invention discloses an electrolytic cell for electrolysis preparation of tetramethylammonium hydroxide. According to the electrolytic cell, a ruthenium dioxide titanium substrate is used as an anode, stainless steel is used as a cathode, a cell body is made of a polytetrafluoroethylene material, and a perfluorocartankylic acid / sulfonic acid composite ionic membrane is used as a cation exchangemembrane; and / or a perfluorosulfonic acid ion membrane is used as an anion exchange membrane. The cleaning agent 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, in particular to the technical field of electrolytic chemistry, and relates to a preparation method of electronic grade tetramethylammonium hydroxide. Background technique [0002] Tetramethylammonium hydroxide, also known as tetramethylammonium hydroxide, has a structural formula of (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 that of inorganic bases NaOH and KOH. [0003] As tetramethylammonium hydroxide products on the market, it is mainly divided into two categories: industrial grade and electronic grade. Electronic grade tetramethylammonium hydroxide is a colorless and transparent mixture of tetramethylammonium hydroxide and water. Typically, tetramethylammonium hydroxide is formulated as 10% (wt%) and 25% (wt%) aqueous solutions. As measured by Toyo Chemical Co., Ltd., ...

Claims

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Application Information

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IPC IPC(8): C25B3/00C25B9/08C25B11/06
CPCC25B3/00
Inventor 刘颂军孙炜孔星
Owner CANGZHOU SUNHEAT CHEM
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