Method for purifying organic amine electroplating additive

A technology of electroplating additives and purification methods, applied in the directions of organic chemistry, chemical instruments and methods, preparation of organic compounds, etc., to achieve good adaptability and market prospects, reduced emissions, and reduced costs.

Active Publication Date: 2013-05-15
SHANGHAI SINYANG SEMICON MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually, EDI technology is used for the production of high-purity water. In the Chinese patent CNCN201770477U, an EDI production device for preparing ultra-clean and high-purity H2O2 was invented. In addition, In the Chinese patent CN101993387A, a method combining rectification and EDI is used to purify electronic-grade N,N-dimethylformamide, but there is no relevant literature report on its application in the purification of organic amine electroplating additives

Method used

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  • Method for purifying organic amine electroplating additive
  • Method for purifying organic amine electroplating additive
  • Method for purifying organic amine electroplating additive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Take 100kg of industrial-grade TMAH pentahydrate, use ultrapure water to prepare a 25% concentration of TMAH solution, use a microfiltration membrane with a pore size of 2 μm to filter the solution to obtain a clear and transparent liquid, put the filtrate into a PP material storage tank, and use a raw material pump 21 The TMAH is input into the electrodeionization device 15, and the purification chamber 7 is equipped with a commercial brand D261 strong basic styrene-based anion exchange resin and Amberlite252Na strong acidic styrene-based cation exchange resin, and the ratio of the anion and cation exchange resins is 2:3 (V: V), cation exchange membrane 11 and anion exchange membrane 12 are polyethylene sulfonic acid type cation membrane 3361W polyethylene tertiary ammonia type anion membrane 3362W (Shanghai Chemical Water Treatment Plant), turn on the DC power supply, operate at constant voltage, and set the initial voltage 70V, conduct electrodeionization operation, c...

Embodiment 2

[0041] Process conditions and equipment are the same as in Example 1, except that the cation-exchange membrane 11 and anion-exchange membrane 12 in the EDI device 15 are changed into ethylene-propylene rubber homogeneous cationic membrane KM ethylene-propylene rubber homogeneous anion membrane AM (Shandong Tianwei membrane Co., Ltd.), when the EDI operation reaches 60 minutes, the anion and cation concentration of the sample is monitored and meets the SEMI standard. As shown in Table 2, the concentration of all metal ions is lower than 2-10ppb, the concentration of chloride ion is lower than 0.1ppm, and the concentration of carbonate Ions below 100ppm. The concentration of TMAH obtained by acid-base titration is 21.67%. Without considering other factors such as electrolytic separation of water, the recovery rate of TMAH can reach 86.7%.

Embodiment 3

[0043] Process condition and equipment are the same as embodiment 2, the difference is that the ion exchange resin in the EDI unit 15 uses JK204 strong base gel type anion exchange resin and D001 macroporous strongly acidic styrene cation exchange resin to be packed in the mixed bed mode instead Purification chamber 7, the ratio of anion exchange resin and cation exchange resin in purification chamber 7 is 2:3 (V:V). When the reaction reaches 60min, take a sample for inspection. After testing, as shown in Table 2, after concentration conversion, all metal ion concentrations are lower than 2-10ppb, chloride ion concentrations are lower than 0.1ppm, and carbonate ions are lower than 100ppm. SEMI standard. The concentration of TMAH at this time was determined to be 21.34% by acid-base titration. Without considering other factors such as electrolytic separation of water, the recovery rate of TMAH was calculated to reach 85.4%.

[0044] From the results of the above examples, it c...

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Abstract

The invention discloses a method for purifying an organic amine electroplating additive. Anion and cation impurities in the organic amine electroplating additive are eliminated by using an electric deionization device; end plates are respectively arranged on two ends of the electric deionization device; cathodes and anodes which are connected with a direct-current power supply are respectively arranged on the end plates; a plurality of purifying chambers and concentrated water chambers are sequentially and alternatively arranged in parallel between two end plates; each purifying chamber and the concentrated water chamber are respectively isolated from each other through cation exchange membranes or anion exchange membranes; the purifying chambers are filled with ion exchange resin; the concentrated water chamber and an electrode water chamber are respectively filled with 0.3-1% organic ammonium salt solutions; the flow of the purifying chamber is 1-100L / h; the flows of the concentrated water chamber and the electrode water chamber are 1-100L / h; the voltage of the direct-current power supply is 0-100V; the voltage is constant and the solution temperature is kept be at 20-70 DEG C in the purification process; and the recovery rate of the organic amine electroplating additive after being purified is greater than 80%. The method for purifying the organic amine electroplating additive, disclosed by the invention, is simple in process and easy to control, and the purification degree can achieve the fine electronic grade standard.

Description

technical field [0001] The invention relates to a method for purifying organic amine compounds, in particular to a method for purifying organic amine electroplating additives, mainly aimed at the removal of metal ion impurities and anion impurities in industrial-grade and electronic-grade organic amine electroplating additives. Background technique [0002] Organic amine electroplating additives refer to the key additives used in high-purity copper sulfate or high-purity copper methanesulfonate electroplating, such as: triethanolamine, triisopropanolamine, diglycolamine, triethylenediamine, N, N-diethylpropynylamine, tetramethylammonium hydroxide, etc. Its general formula is as follows: [0003] [0004] R 1 -R 3 Represents H or alkyl, alkenyl, alkynyl, alkoxy, alkanol, acetyl, benzyl, etc. with 1-10 carbon chains. [0005] Organic amine electroplating additives, such as tetramethylammonium hydroxide (TMAH) and triethanolamine, belong to organic bases and have a ver...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/84C07C213/10C07C211/63
Inventor 孙江燕梁重时任发强
Owner SHANGHAI SINYANG SEMICON MATERIALS
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