Crystallization tower for purifying phosphoric acid

A crystallization tower, phosphoric acid technology, applied in crystallization separation, phosphorus compounds, inorganic chemistry and other directions, can solve the problems of low yield of purified phosphoric acid, complicated operation steps, inconvenient continuous production, etc., to improve the separation and purification effect, continuous and stable The effect of production and easy processing

Active Publication Date: 2012-07-18
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ordinary jacketed crystallizers and coiled cooling crystallizers pass the cooling medium into the jacket or coiled tubes, and exchange heat through the partition wall to cool and crystallize the phosphoric acid solution. The heat exchange surface of such cooling crystallizers is easy to scale, resulting in heat transfer The effect is poor and the production capacity is small. In addition, although the purity requirements can be achieved after multiple recrystallization operations, the product yield is low and the operation steps are complicated, so it is inconvenient to use in industrial production.
The layered crystallizer and liquid film crystallization tower are used to purify phosphoric acid. The phosphoric acid material circulates in the layered crystallizer and liquid film crystallization tower for crystallization and purification. operating under low conditions, and requires multiple operations to meet the purity requirements, which is not convenient for continuous production, and the yield of purified phosphoric acid is still not high

Method used

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  • Crystallization tower for purifying phosphoric acid
  • Crystallization tower for purifying phosphoric acid
  • Crystallization tower for purifying phosphoric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In this embodiment, the structure of the crystallization tower for purifying phosphoric acid is as follows figure 1 As shown, it includes a tower body 1, an agitator 2, a heater 9 and a driving mechanism.

[0038] The tower body 1 is a cylindrical body, and its bottom and periphery are made of polytetrafluoroethylene. The tower body 1 is divided into a cooling crystallization section a, a separation and purification section b, and a crystal melting section c. The cooling crystallization section is located in the tower The upper part of the tower body has a length of 0.2m. The crystal melting section is located in the lower part of the tower body, and its length is 0.15m. The separation and purification section is located between the cooling crystallization section and the crystal melting section, and its length is 1m. There is a feed inlet 7 and a refrigerant inlet 3, the refrigerant inlet is located above the feed inlet 7, the upper part of the cooling crystallization ...

Embodiment 2

[0059] In this embodiment, the structure of the crystallization tower for purifying phosphoric acid is as follows figure 1 As shown, it includes a tower body 1, an agitator 2, a heater 9 and a driving mechanism. The difference from Embodiment 1 is that the tower body 1 is inclined by 5° relative to the vertical direction.

[0060] Use the crystallization tower described in this embodiment to prepare electronic-grade phosphoric acid with the same industrial phosphoric acid as in Example 1, and the process steps are as follows:

[0061] ① Arsenic removal

[0062] Add phosphorus pentasulfide to industrial phosphoric acid at a temperature of 40°C, and react for 100 minutes at 40°C under normal pressure under stirring (500r / min). After expiry, add the diatomite of phosphoric acid quality 8%, leave standstill 20min, then suction filtration, drip hydrogen peroxide in the phosphoric acid solution obtained by suction filtration, the dripping amount of hydrogen peroxide is 0.5% of des...

Embodiment 3

[0071] In this embodiment, the structure of the crystallization tower for purifying phosphoric acid is as follows figure 1 As shown, it includes a tower body 1, an agitator 2, a heater 9 and a driving mechanism. The difference from Embodiment 1 is that the tower body 1 is inclined 20° relative to the vertical direction.

[0072] Use the crystallization tower described in this embodiment to prepare electronic-grade phosphoric acid with the same industrial phosphoric acid as in Example 1, and the process steps are as follows:

[0073] ① Arsenic removal

[0074] Add phosphorus pentasulfide to industrial phosphoric acid at a temperature of 60°C, and react at normal pressure at 60°C for 60 minutes under stirring (500r / min), the amount of phosphorus pentasulfide added is twice the molar amount of arsenic contained in industrial phosphoric acid, and the reaction time After expiry, add the diatomite of phosphoric acid quality 10%, leave standstill 30min, then suction filtration, dri...

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Abstract

The invention relates to a crystallization tower for purifying phosphoric acid. The crystallization tower comprises a tower body, one stirrer, a heater and a driving mechanism, wherein the tower body is divided into a cooling crystallization section, a separating purification section and a crystal melting section; the cooling crystallization section is arranged at the upper part of the tower body; the crystal melting section is arranged at the lower part of the tower body; the separating purification section is arranged between the cooling crystallization section and the crystal melting section; a feeding hole and a coolant inlet are arranged at the lower part of the cooling crystallization section of the tower body; the coolant inlet is arranged above the feeding hole; the upper part of the cooling crystallization section of the tower body is provided with a raffinate and coolant discharge hole; the bottom of the crystal melting section of the tower body is provided with a purified phosphoric acid outlet; the main body part of the stirrer is arranged in the tower body; one end of the stirrer extends out of the tower body and is connected with a speed reducer of the driving mechanism; and the heater is arranged on the tower body and is positioned on the crystal melting section of the tower body.

Description

technical field [0001] The invention belongs to a phosphoric acid purification device, in particular to a crystallization tower for purifying phosphoric acid by adopting a fusion crystallization method. Background technique [0002] The devices for purifying phosphoric acid by melt crystallization include ordinary jacketed crystallizers, coil cooling crystallizers, layer crystallizers and liquid film crystallization towers. Ordinary jacketed crystallizers and coiled cooling crystallizers pass the cooling medium into the jacket or coiled tubes, and exchange heat through the partition wall to cool and crystallize the phosphoric acid solution. The heat exchange surface of such cooling crystallizers is easy to scale, resulting in heat transfer The effect is poor, and the production capacity is small. In addition, although the purity requirement can be achieved through multiple recrystallization operations, the product yield is low and the operation steps are complicated, which i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D9/00C01B25/234
Inventor 李军王保明罗建洪金央周堃齐亚兵马春磊
Owner SICHUAN UNIV
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