Synthesis method and equipment for tetramethylammonium hydroxide

A technology of tetramethylammonium hydroxide and synthesis method, which is applied in the direction of electrodes, electrolysis process, electrolysis components, etc., can solve the problems of short service life of graphite anode and low efficiency of electrolysis current

Active Publication Date: 2020-11-20
信联电子材料科技股份有限公司
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  • Abstract
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Problems solved by technology

[0005] For this reason, the present invention proposes a synthetic method and equipment for tetramethylammonium hydroxide, which can solve t

Method used

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  • Synthesis method and equipment for tetramethylammonium hydroxide
  • Synthesis method and equipment for tetramethylammonium hydroxide

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preparation example Construction

[0031] Such as figure 1 Shown, a kind of synthetic method for tetramethylammonium hydroxide comprises the following steps:

[0032] (1) butadiene derivatives are dissolved in an organic solvent to prepare an electrode electrolyte, a graphite electrode is used as a reaction electrode, platinum is used as a counter electrode, and a silver / silver chloride electrode is used as a reference electrode and put into the electrode electrolyte, Power on at -0.3V (vs.Ag / Ag+) for polymerization. After the reaction is over, a yellow film is formed on the surface of the graphite electrode to obtain a modified graphite electrode. Take it out and dry it, and place it in the anode chamber;

[0033] (2) The anode chamber and the cathode chamber are separated by a cation exchange membrane, and a cathode is placed in the cathode chamber;

[0034] (3) Connect the current between the modified graphite electrode and the cathode, use tetramethylammonium chloride solution as raw material, pump it into...

Embodiment 1

[0050] Dissolve 1,1,4,4-tetrachloro,2,3-difluorobutadiene and lithium tetrafluoroborate in tetrahydrofuran to prepare electrode electrolyte, use graphite electrode as reaction electrode, platinum as counter electrode, silver / The silver chloride electrode is used as a reference electrode and placed in the electrode electrolyte, and is energized at -0.3V (vs.Ag / Ag+) for 1 hour for polymerization. After the reaction is completed, a yellow film is formed on the surface of the graphite electrode to obtain a modified graphite electrode. , take it out and dry it, and place it in the anode chamber.

[0051] A stainless steel plate is placed in the cathode chamber as the cathode, and the anode chamber and the cathode chamber are separated by a cation exchange membrane. Connect the current between the modified graphite electrode and the cathode, use tetramethylammonium chloride solution as the raw material, pump it into the anode chamber through the anolyte raw material tank and the an...

Embodiment 2

[0054] Except that 1,1,4,4-tetrachloro,2,3-difluorobutadiene was replaced by hexachlorobutadiene, the rest was the same as that of Example 1.

[0055] During this synthesis process, the current efficiency of electrolysis was 93.0%, and the lifetime of the modified graphite electrode was 91 days.

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Abstract

The invention discloses a synthetic method and equipment for tetramethylammonium hydroxide. The synthesis method comprises the following steps: dissolving a butadiene derivative and a supporting electrolyte in an organic solvent to prepare an electrode electrolyte, electrifying a graphite electrode under the electrode electrolyte to form a yellow polymer film on the surface of the graphite electrode to obtain a modified graphite electrode, and applying the modified graphite electrode to an anode chamber of an electrolytic cell. According to the invention, a layer of protective film is formed on the surface of the graphite electrode, so that the oxidation of the graphite electrode is inhibited, the corrosion speed of the graphite electrode is reduced, the current efficiency of electrolysisis improved, and good current efficiency and electrode service life can be obtained even at a high electrolyte circulation rate.

Description

technical field [0001] The invention relates to a synthesis method and equipment for organic compounds, in particular to a synthesis method and equipment for tetramethylammonium hydroxide. Background technique [0002] Tetramethylammonium hydroxide (TMAH) is a strong base of equal strength to caustic. Because of its strong alkalinity and no residue after thermal decomposition, especially no conductive ionic substances, it is widely used in the field of electronics industry. With the continuous development of large-scale integrated circuits, the demand for high-purity electronic-grade TMAH is increasing, but the traditional method of preparing TMAH has defects such as high cost and high content of impurity ions. [0003] At present, the preparation methods of TMAH mainly include: precipitation method, ion exchange resin method, addition method, ion membrane method and ion membrane electrolysis method. The precipitation method has the disadvantages of high process cost and l...

Claims

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Application Information

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IPC IPC(8): C25B3/00C25B11/12
CPCC25B3/00
Inventor 刘颂军孙炜刘新雨
Owner 信联电子材料科技股份有限公司
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