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Method for preparing electronic grade phosphoric acid by use of septum type crystallization process

An electronic-grade phosphoric acid and crystallization technology, which is applied in the fields of phosphorus compounds, chemical instruments and methods, and inorganic chemistry, can solve the problems of low efficiency, complex electronic-grade phosphoric acid devices, and large energy consumption, so as to increase the area and reduce energy consumption , the effect of improving the crystallization efficiency

Pending Publication Date: 2014-05-07
GUANGXI MINGLI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The device for producing electronic-grade phosphoric acid in this utility model is complicated, consumes a lot of energy, and has low efficiency

Method used

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  • Method for preparing electronic grade phosphoric acid by use of septum type crystallization process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Firstly, beat the orthophosphoric acid with a temperature of 29°C and a concentration of 86% to the 1 / 2 liquid level of the crystal grid of the clapboard crystallizer, 2000kg of acid in 4 grids, and then inject -15°C brine into the cold and hot medium grids The phosphoric acid in the crystal lattice is cyclically cooled, and then the phosphoric acid semi-crystal seed is added into the crystal lattice from the seeding port according to 5‰ of the original phosphoric acid weight, so that the phosphoric acid semi-crystal seed induces phosphoric acid crystallization, and the phosphoric acid crystal begins to grow slowly , when the thickness of the crystalline layer gradually increases to 5cm, stop adding brine to the cold and hot medium cells, open the brine drain valve and liquid phase drain valve to drain brine and liquid phase, liquid phase dephosphoric acid hydration process, let stand for 30min to crystallize The residual liquid phase on the surface was dripped off, and ...

Embodiment 2

[0042] First, beat the orthophosphoric acid with a temperature of 29.5°C and a concentration of 87% to the 3 / 4 liquid level of the crystal lattice of the clapboard crystallizer, 3000kg of acid in 4 lattices, and then pour the brine at -8°C into the cold and hot medium lattice The phosphoric acid in the crystal lattice is cyclically cooled, and then the phosphoric acid semi-crystal seed is added into the crystal lattice from the seeding port according to 8‰ of the original phosphoric acid weight, so that the phosphoric acid semi-crystal seed induces phosphoric acid crystallization, and the phosphoric acid crystal begins to grow slowly. , when the thickness of the crystalline layer gradually increases to 5.5cm, stop adding brine to the hot and cold medium grid, open the brine drain valve and liquid phase drain valve to drain brine and liquid phase, liquid phase dephosphoric acid hydration process, let stand for 35min The residual liquid phase on the crystal surface was dripped of...

Embodiment 3

[0047] First, the outlet valve of the circulating acid of the acid adjustment tank is opened, and the molten acid sample with a temperature of 30°C and a concentration of 88% produced in Examples 1 and 2 is beaten to the crystal lattice 4 / 5 liquid of the clapboard crystallizer. At the location, 4 grids of acid total 3362kg, and then put -3 ℃ brine into the cold and hot medium grid to circulate and cool the phosphoric acid in the crystal grid, and then add semi-crystal seeds of phosphoric acid according to 10‰ of the weight of the original phosphoric acid Add the mouth into the crystal grid, so that the phosphoric acid semi-crystal seed induces phosphoric acid crystallization, and the phosphoric acid crystal begins to grow slowly. When the thickness of the crystal layer gradually increases to 6cm, stop adding brine to the cold and hot medium grid, open the brine drain valve and drain The phase valve is used to drain the brine and remove the liquid phase, and let it stand for 40 ...

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Abstract

The invention discloses a method for preparing electronic grade phosphoric acid by use of septum type crystallization process. The principle that the crystallization temperature of impurities in phosphoric acid is lower than that of pure phosphoric acid and the melting temperature of impurities is higher than that of pure phosphoric acid is utilized, that is, the crystallization speed of pure phosphoric acid is higher than that of the impurities during cooling crystallization, and the precipitation speed of the impurities is higher than that of pure phosphoric acid during melting; a septum type crystallizer is adopted to enable phosphoric acid to be crystallized on a septum surface, the unit crystallization area is increased and the crystallization efficiency is improved; a crystal washing device is arranged in the septum type crystallizer and used for spraying and washing residual liquid phase on the surface of a crystal column and in crystallization lattices, and a condition that the liquid phase with high impurity content and pure crystals are mixed to cause the quality of a product to be deteriorated is avoided; hot water produced by phosphoric acid production enterprises is used as a heat source for melting crystals, so that the energy consumption is greatly reduced and good economic benefit is achieved.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemical industry and relates to the preparation of electronic-grade phosphoric acid by a partition type crystallization method. Background technique [0002] Electronic-grade phosphoric acid belongs to high-purity phosphoric acid, which is widely used in large-scale integrated circuits and thin-film liquid crystal displays (TFT-LCD) [0003] It is mainly used in the cleaning and etching of chips in the microelectronics industry. Its purity and cleanliness have a great influence on the yield, conductivity and reliability of electronic components. Those with lower purity are mainly used for cleaning liquid crystal panel components. The ones with higher purity are mainly used for cleaning and etching in the production process of electronic wafers. Since insoluble solid particles or metal ions may conduct current between tiny circuits and make them short circuit, electronic-grade phosphoric acid is...

Claims

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Application Information

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IPC IPC(8): C01B25/234
Inventor 林军吴小海苏杰文王文营
Owner GUANGXI MINGLI CHEM
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