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A process of coupling crystallization-electrodialysis-reverse osmosis to prepare electronic-grade phosphoric acid with different purity

A technology of electrodialysis and reverse osmosis, which is applied in the direction of phosphorus compounds, inorganic chemistry, non-metallic elements, etc., can solve the problems of relatively strict production process requirements, and achieve the effects of easy operation, pollution reduction, and no secondary pollution

Active Publication Date: 2015-11-11
WUHAN XINGUI TECH QIANJIANG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Li Tianxiang and others also proposed a production method of high-purity orthophosphoric acid crystals, which is disclosed by Chinese patent CN200810068736.7. In the process of crystallization and recrystallization, the method of gradient cooling is adopted, which can effectively inhibit the secondary nucleation in the process of crystallization and recrystallization , to obtain hemihydrate phosphoric acid crystals or orthophosphoric acid crystals with a regular appearance and an average particle size of more than 0.5mm. After testing, the crystallized products reach the MOS level, and the recrystallized products meet the BV-Ⅰ electronic grade phosphoric acid index requirements, but the production process requires more harsh

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  • A process of coupling crystallization-electrodialysis-reverse osmosis to prepare electronic-grade phosphoric acid with different purity
  • A process of coupling crystallization-electrodialysis-reverse osmosis to prepare electronic-grade phosphoric acid with different purity
  • A process of coupling crystallization-electrodialysis-reverse osmosis to prepare electronic-grade phosphoric acid with different purity

Examples

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Embodiment 1

[0032] In this example, a process flow of coupling crystallization-electrodialysis-reverse osmosis to prepare electronic-grade phosphoric acid with different purity is shown in figure 1 , including the following steps:

[0033] (1) Use crystallization to separate and remove impurities from industrial-grade phosphoric acid: such as figure 2 As shown, the crystallizer adopts a partitioned cylindrical vertical device with a length-to-diameter ratio of 8:1. The cold source uses industrial ethylene glycol, which is placed in a low-temperature coolant circulation pump to freeze to -12°C. The heat source uses industrial ethylene glycol. , placed in a water bath and heated to 45°C;

[0034] 1.1 Turn on the constant flow pump, transport industrial-grade phosphoric acid to the upper pipe of the crystallizer, ensure that the crystallizer is filled, then turn off the constant flow pump, turn on the low-temperature cooling liquid circulation pump, and continuously carry out refrigeration...

Embodiment 2

[0046] In this embodiment, a process of coupling crystallization-electrodialysis-reverse osmosis to prepare electronic-grade phosphoric acid of different purity is roughly the same as that of Example 1, except that:

[0047] (1) During the purification process of the electrodialysis method, the electrode is a platinum electrode, the temperature of the electrodialysis is 20°C, and the current density of the electrodialysis is 30A / dm 2 , the anion exchange membrane is polyvinyl chloride, and the cation exchange membrane is a polyethylene homogeneous ion exchange membrane;

[0048] (2) During the purification process of the reverse osmosis method, the mass concentration of phosphoric acid in the phosphoric acid solution to be treated is 15%, the operating pressure of the reverse osmosis is 0.5MPa, the reverse osmosis membrane is a polyamide permeable membrane, and the phosphoric acid The mass concentration of phosphoric acid in the concentrate is 78%.

[0049] In this example, t...

Embodiment 3

[0051] In this embodiment, a process of coupling crystallization-electrodialysis-reverse osmosis to prepare electronic-grade phosphoric acid of different purity is roughly the same as that of Example 1, except that:

[0052] (1) During the purification process of the electrodialysis method, the electrode is a ruthenium-coated titanium plate electrode, the temperature of the electrodialysis is 60°C, and the current density of the electrodialysis is 1A / dm 2 , the anion exchange membrane is a polytetrafluoroethylene homogeneous ion exchange membrane, and the cation exchange membrane is a sulfonic acid membrane;

[0053] (2) During the purification process of the reverse osmosis method, the mass concentration of phosphoric acid in the phosphoric acid solution to be treated is 1%, the operating pressure of the reverse osmosis is 10MPa, and the reverse osmosis membrane is a polyimide permeable membrane. The mass concentration of phosphoric acid in the phosphoric acid concentrated so...

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Abstract

The invention belongs to the technical field of phosphoric acid purification and provides a process for preparing electronic grade phosphoric acids with different purities by crystallization, electroosmosis and reverse osmosis coupling. According to the process disclosed by the invention, the defects of a single separation and purification technology are made up by coupling various separation and purification technologies and the electronic grade phosphoric acid with the purity greater than 99.99 percent can be effectively prepared; besides, a product 1 obtained by purifying treatment through a crystallization method and a product 2 obtained by purifying treatment through a crystallization and electroosmosis method respectively meet the standard requirements of MOS (Metal Oxide Semiconductor) grade electronic grade phosphoric acid and different demands on application of the electronic grade phosphoric acids can be met. The process disclosed by the invention has the advantages of mild process conditions, less investment, low energy consumption, easiness for operation, good safety and no secondary pollution.

Description

technical field [0001] The invention belongs to the technical field of phosphoric acid purification, and in particular relates to a process for preparing electronic-grade phosphoric acid with different purity by coupling crystallization-electrodialysis-reverse osmosis. Background technique [0002] Phosphoric acid can be divided into fertilizer grade, industrial grade, food grade, pharmaceutical grade and high-purity grade according to the content of impurities. Different grades of phosphoric acid are used in different fields. Electronic-grade phosphoric acid is high-purity phosphoric acid, which is widely used in wet cleaning and wet etching of chips in the microelectronics industry. Its purity and cleanliness have a great impact on the yield, electrical performance and reliability of electronic components. [0003] With the continuous improvement of IC integration, the control of the content of insoluble solid particles and most metal ions in the reagent is more stringent,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/234
Inventor 覃远航李想冀少卿王存文王为国吕仁亮段晓玲
Owner WUHAN XINGUI TECH QIANJIANG CO LTD