Device and method for recycling aluminum etching solution

An aluminum etching and material liquid technology, applied in the field of electronic chemicals, can solve the environmental impact of waste discharge, ethanol residue in phosphoric acid, reduce the concentration of phosphoric acid, etc., to simplify the recycling process, improve the quality concentration and purity, Effect of Simplified Recycling Process

Active Publication Date: 2020-04-17
湖北兴福电子材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, domestic waste acid treatment methods mainly include: concentration method, neutralization method, roasting method, extraction method, ion exchange method, etc., none of which can effectively recycle waste acid and avoid the generation of waste
Not only increases the production cost of semiconductors and panels, but also the discharge of waste will have an impact on the environment
[0004] Chinese patent CN200510075397 proposes a method for purifying phosphoric acid by combining fractionation and esterification. First, the nitric acid is vaporized and separated, and the mixture of phosphoric acid and acetic acid is converted into acetate by ethanol esterification, thereby separating acetic acid and phosphoric acid. No waste liquid is generated, and phosphoric acid in the aluminum etching solution can be effectively separated. However, in the process of acetic acid separation, this method first adopts negative pressure distillation to separate most of the acetic acid, and then uses a small amount of acetic acid in ethanol and phosphoric acid to form acetate, which is separated Phosphoric acid, this process is not only complicated, but also reduces the concentration of phosphoric acid, and some ethanol will remain in phosphoric acid, affecting product quality
This method can completely separate phosphoric acid, acetic acid, and nitric acid, and no waste acid is produced, but this method is complex in process, and has low yield and high energy consumption in the process of phosphoric acid crystallization, melting and purification, and cannot be applied to industrial production on a large scale.

Method used

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  • Device and method for recycling aluminum etching solution

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Effect test

Embodiment 1

[0031] Such as figure 1 As shown, a device for recovering and reusing aluminum etching solution includes a waste acid storage tank 1, which is connected to a reactor 3 feed line, and the reactor 3 is also connected to a phosphorus pentoxide feed pipeline; the reactor 3 outlet Connected to the evaporator 5, the outlet of the evaporator is connected to the evaporation separator 6, the gas outlet of the evaporation separator is connected to the exhaust gas condenser 7 and the exhaust gas separator 8 in turn, and the liquid outlet of the evaporation separator is connected to the phosphoric acid stripping tower 9, Then connect the phosphoric acid mixing tank 11 and the phosphoric acid storage tank 13 in sequence; the lower part of the phosphoric acid stripping tower is provided with a nitrogen inlet pipe.

[0032] In a preferred solution, a jacketed heat exchanger is arranged outside the reactor. In another preferred solution, a nitrogen feed line is also arranged on the phosphoru...

Embodiment 2

[0039] The method for recycling the aluminum etching solution by using the above-mentioned device comprises the following steps:

[0040](1) The aluminum etching solution in the waste acid storage tank is fed into the reactor, and reacts with phosphorus pentoxide to increase the concentration of phosphoric acid in the mixed acid to 86% to 88%, and it is added through the high-purity nitrogen gas on the phosphorus pentoxide pipeline For the pipeline, the nitrogen pressure is controlled at 10kpa to 20kpa, and the phosphorus pentoxide is dispersed and protected by nitrogen sealing;

[0041] (2) After the reaction, the mixed acid is transported to the evaporator to heat up, and the temperature is controlled at 80°C to 85°C. The heated mixed acid enters the evaporator separator in a negative pressure state for gas-liquid separation. The negative pressure is -0.15Mpa, and the gaseous nitric acid and Acetic acid enters the exhaust gas condenser from the top of the gas-liquid separato...

Embodiment 3

[0045] Carry out the method for recycling aluminum etching solution with device among the embodiment 1, may further comprise the steps:

[0046] (1) The aluminum etching solution in the waste acid storage tank is fed into the reactor, and reacts with phosphorus pentoxide to increase the concentration of phosphoric acid in the mixed acid to 80% to 83%, and it is added through the high-purity nitrogen gas on the phosphorus pentoxide pipeline Pipeline, disperse phosphorus pentoxide and protect it with nitrogen blanketing;

[0047] (2) After the reaction, the mixed acid is transported to the evaporator to heat up, and the temperature is controlled at 90°C to 95°C. The heated mixed acid enters the evaporator separator in a negative pressure state for gas-liquid separation. The negative pressure is -0.05Mpa, and the gaseous nitric acid and Acetic acid enters the exhaust gas condenser from the top of the gas-liquid separator, cools to 60°C and becomes liquid, enters the mixed acid st...

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Abstract

The invention discloses a device and method for recycling an aluminum etching solution. The device comprises a waste acid storage tank, wherein the waste acid storage tank is connected to a feeding pipeline of a reaction kettle; the reaction kettle is also connected with a phosphorus pentoxide feeding pipeline; a discharge hole of the reaction kettle is connected to an evaporator; a discharge holeof the evaporator is connected to an evaporation separator; a gas outlet of the evaporation separator is sequentially connected with an exhaust gas condenser and an exhaust gas separator; a liquid outlet of the evaporation separator is connected to a phosphoric acid stripping tower and then is sequentially connected with a phosphoric acid blending kettle and a phosphoric acid storage tank; and anitrogen introducing pipeline is arranged on the lower part of the phosphoric acid stripping tower. By adopting the device and method disclosed by the invention, phosphoric acid in the waste aluminumetching solution can be effectively separated from nitric acid and acetic acid, the nitric acid and the acetic acid can be recycled for producing the etching solution, and industrial phosphoric acid of various concentrations can be blended according to the requirements, so that the waste is changed into valuable.

Description

technical field [0001] The invention belongs to the field of electronic chemicals, and in particular relates to a device and method for recycling aluminum etching solution in a semiconductor factory. Background technique [0002] Aluminum etchant is a formula-type electronic chemical used to etch and remove panel aluminum or aluminum alloy in the TFT-LCD panel manufacturing process. Its main composition is phosphoric acid and a small amount of nitric acid, acetic acid, and additives. Aluminum etching solution will produce a large amount of waste liquid containing phosphoric acid, nitric acid, acetic acid and other impurities after use. Due to the high cost and difficulty of processing waste liquid containing phosphorus and acid, most semiconductor and panel manufacturers outsource the treatment. [0003] At present, domestic waste acid treatment methods mainly include: concentration method, neutralization method, roasting method, extraction method, ion exchange method, etc.,...

Claims

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Application Information

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IPC IPC(8): C23F1/46C01B25/234
CPCC23F1/46C01B25/234
Inventor 李少平杨着郭岚峰蔡步林杨阳万永洲
Owner 湖北兴福电子材料股份有限公司
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