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Method for preparing electronic grade tetramethylammonium hydroxide by continuous method

A tetramethylammonium hydroxide, electronic-grade technology, applied in electrolysis process, electrolysis components, electrolysis organic production, etc., can solve the problems of pollution, consumption of silver oxide, inability to scale production, etc., and achieve high product purity and power utilization rate High and reduce the effect of industrial three wastes

Active Publication Date: 2012-04-04
镇江润晶高纯化工科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the silver oxide method is used to produce tetramethylammonium hydroxide, that is, the reaction of tetramethylammonium chloride and silver oxide produces tetramethylammonium hydroxide , the defect of the process route of this method is: 1, can only produce intermittently, can't scale production; 2, need to consume precious silver oxide, and cost is higher; ions, making tetramethylammonium hydroxide contaminated by silver ions
4. The purity of the generated tetramethylammonium hydroxide is low, the concentration of each metal ion in it is 50 ppb, and the concentration of each anion is greater than 550 ppb

Method used

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  • Method for preparing electronic grade tetramethylammonium hydroxide by continuous method
  • Method for preparing electronic grade tetramethylammonium hydroxide by continuous method
  • Method for preparing electronic grade tetramethylammonium hydroxide by continuous method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The electrode material of the anode plate 9 is titanium, the electrode material of the cathode plate 8 is nickel, the plate is coated with oxygen and chlorine evolution, and the current density is 1000 A / ㎡. The electrolyte in the two adjacent chambers of the cathode chamber 1, the first cathode intermediate chamber 2, the second cathode intermediate chamber 3, and the anode chamber 4 are all externally circulated by the circulation pump 13, and the anode chamber 4 itself uses the circulation pump 13. Carry out internal circulation. Concentration is the saline solution of 50% tetramethylammonium bicarbonate in the anode chamber 4, is the tetramethylammonium hydroxide that concentration is 20% in the second cathode intermediate chamber 3, is concentration in the first cathode intermediate chamber 2. 3% tetramethylammonium hydroxide, the concentration of 30% tetramethylammonium hydroxide in the cathode chamber 1, the current efficiency is 70%.

[0022] By connecting the c...

Embodiment 2

[0024] The electrode material of the anode plate 9 is titanium, the electrode material of the cathode plate 8 is graphite, the plate is coated with oxygen and chlorine evolution, and the current density is 1500 A / ㎡. The pump circulation mode of the electrolyte in each chamber is the same as that of Embodiment 1. Concentration is 40% tetramethylammonium bicarbonate solution in the anode chamber 4, concentration is 10% tetramethylammonium hydroxide in the second cathode intermediate chamber 3, and concentration is 10% in the first cathode intermediate chamber 2 Tetramethylammonium hydroxide, in the cathode compartment 1 is the tetramethylammonium hydroxide concentration of 15%, and the current efficiency is 90%.

[0025] Connecting the current between the two plates can continuously electrolyze and prepare electronic-grade tetramethylammonium hydroxide. The concentration of each metal ion in the prepared electronic-grade tetramethylammonium hydroxide is less than 10 ppb, and the...

Embodiment 3

[0027] The electrode material of the anode plate 9 is titanium, the electrode material of the cathode plate 8 is graphite, the plate is coated with oxygen and chlorine evolution, and the current density is 2000 A / ㎡. The pump circulation mode of the electrolyte in each chamber is the same as that of Embodiment 1. Concentration is 5% tetramethylammonium bicarbonate solution in the anode chamber 4, concentration is 1% tetramethylammonium hydroxide in the second cathode intermediate chamber 3, and concentration is 4% in the first cathode intermediate chamber 2 Tetramethylammonium hydroxide, the concentration is 5% tetramethylammonium hydroxide in the cathode chamber 1, and the current efficiency is 83%.

[0028] Connecting the current between the two plates can continuously electrolyze and prepare electronic grade tetramethylammonium hydroxide. The concentration of each metal ion in the prepared electronic grade tetramethylammonium hydroxide is less than 10 ppb (see Table 1), and ...

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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

technical field [0001] The invention relates to a method for preparing tetramethylammonium hydroxide, in particular to a method for preparing electronic-grade tetramethylammonium hydroxide by using a continuous electrolysis method with tetramethylammonium salt as a raw material. Background technique [0002] Tetramethylammonium hydroxide (TMAH) is an important industrial and electronic chemical product, and has a wide range of uses in the industrial field, such as a catalyst for the synthesis of organosilicon products, used for polyester polymerization, textiles, plastic products and Leather and other fields. Electronic grade tetramethylammonium hydroxide is mainly used on liquid crystal panels and chips as a developer. [0003] At present, the production of tetramethylammonium hydroxide all adopts the silver oxide method, that is, the reaction of tetramethylammonium chloride and silver oxide generates tetramethylammonium hydroxide. The defect of the process route of this m...

Claims

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Application Information

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IPC IPC(8): C25B3/00C25B9/06C25B9/08C25B9/17C25B9/19
Inventor 赵文洲
Owner 镇江润晶高纯化工科技股份有限公司
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