Device and method for recycling waste acid liquid produced in polycrystalline silicon texturing

A waste acid solution and polysilicon technology, applied in chemical instruments and methods, fluosilicic acid, nitric acid, etc., can solve the problems of increased investment, serious equipment corrosion, and the production of equal volumes of dilute waste acid, etc., to reduce purification costs, The effect of reducing drug costs and stabilizing product indicators

Active Publication Date: 2020-05-19
SUZHOU KZONE EQUIP TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the thermal decomposition of nitric acid and nitrate into nitrogen oxides, it is necessary to increase the tail gas nitrogen oxide purification system and increase investment.
At the same time, the recovery rate of nitric acid is only about 30%, and the equipment is seriously anti-corrosion.
[0007] The fourth is membrane separation. The advantage of membrane separation is small investment and relatively simple device structure. The disadvantage is that it will produce an equal volume of dilute waste acid, and the separation effect for low-concentration metal ions is not good, and the technology is immature
[0008] The fifth is resin adsorption, which is to use special resin for the adsorption treatment of waste acid. Although the special resin adsorption process can achieve the purpose of recycling waste acid without consuming heat energy, its disadvantage is that after the resin adsorption treatment reaches saturation, it will consume at least the same amount of pure water for resin regeneration
As a result, the investment in the pure water system and the wastewater treatment system will be increased, and the residual metal ions in the recovered acid are still about 20%.

Method used

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  • Device and method for recycling waste acid liquid produced in polycrystalline silicon texturing
  • Device and method for recycling waste acid liquid produced in polycrystalline silicon texturing

Examples

Experimental program
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Effect test

Embodiment 1

[0038] This embodiment describes a device for recycling waste acid liquid from polysilicon texturing, such as figure 1As shown, it mainly includes a silica reactor 1, a nitrate reactor 2, a bag filter 3, a rectification tower 10, a first condenser 11, a vacuum buffer tank 13, a concentrated nitric acid storage tank 14, and dilute magnesium nitrate Storage tanks 17, 18, evaporator 19, second condenser 20, reclaimed water buffer tank 21 and concentrated magnesium nitrate storage tank 24 are also provided with some pump valves for pumping and transporting liquid or gas. Wherein, the silica reaction kettle 1, the nitrate reaction kettle 2, the bag filter 3, the rectifying tower 10, the first condenser 11, the vacuum buffer tank 13, and the concentrated nitric acid storage tank 14 are connected successively by pipelines , the dilute magnesium nitrate storage tanks 17, 18 are connected to the rectification tower 10 for collecting the dilute magnesium nitrate remaining at the bottom ...

Embodiment 2

[0046] In particular, this embodiment describes a method for recycling polysilicon texturing waste acid solution, which includes:

[0047] Step 1: Determining the content of nitric acid, hydrofluoric acid and fluorosilicic acid in the waste acid solution of texturing;

[0048] Step 2: After measuring the content of each acid solution, mix and add silicon dioxide into the waste acid solution for texturing, and the ratio of the molar amount of silicon dioxide added to the molar amount of hydrofluoric acid is 1:1, and the reaction is stirred for 30 minutes. React the hydrofluoric acid in it to generate fluosilicic acid and silicon tetrafluoride, and silicon tetrafluoride can be used as a gas to pass through the exhaust channel to the exhaust gas treatment equipment;

[0049] Step 3: Potassium nitrate is added to the mixed acid solution after adding silicon dioxide to react. The molar ratio of potassium nitrate to fluosilicic acid is 2:1. After stirring for 30 minutes, the tempera...

Embodiment 3

[0054] In this example, the waste acid from the polysilicon texturing production line is used, and the content is about 30% of nitric acid, about 3% of hydrofluoric acid, about 5% of fluosilicic acid, and metal ions such as silver ions, aluminum ions, calcium ions, The content of potassium ions, sodium ions, zinc ions, etc. ranges from hundreds of ppb to tens of thousands of ppb, and the processing capacity is 1 ton / day. Waste acid liquid is collected in batches and sent to silica reactor 1 (1 cubic meter), add 24.8 kilograms of silicon dioxide, stir and react for 30 minutes, then send to potassium nitrate reactor (1 cubic meter), add 116.4 kilograms of potassium nitrate , after stirring for 30 minutes, the potassium nitrate reaction kettle is a jacketed stirring reaction kettle. After the reaction is completed, the jacket is fed with cooling water at 5 to 7 degrees Celsius for half an hour, and then passed through a bag filter. Filter through filter 4, the filter residue is p...

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Abstract

The invention relates to a device and a method for recycling waste acid liquid produced in polycrystalline silicon texturing. According to the method, in a secondary chemical reaction precipitation section, hydrofluoric acid is neutralized through a primary reaction, a fluorosilicate precipitate is generated through a secondary reaction, and the precipitate can be sold; in a rectification and purification section, rectification and purification can be performed on dilute nitric acid to generate concentrated nitric acid; the nitric acid is evaporated and concentrated to obtain about 65% of dilute nitric acid through a dehydrating agent reduced-pressure rectification process, and the dilute nitric acid can be directly reused in a texturing liquid system, so the cyclic utilization of nitric acid is achieved, and reagent cost is reduced; and in a dehydrating agent regeneration section, a certain amount of magnesium oxide is added into a solution containing a small amount of dilute magnesium nitrate for neutralization, and then evaporation is carried out so as to obtain high-concentration concentrated magnesium nitrate which can be directly used as a dehydrating agent and applied to therectification and purification section. According to the invention, resource utilization and recycling of waste water and solid waste are realized, the operation cost and production cost of enterprises are further reduced, and the requirements of energy conservation, high efficiency and environmental protection are met.

Description

technical field [0001] The invention relates to the technical field of environmental protection treatment, in particular to the technical field of waste liquid recovery and reuse, in particular to a device and method for recycling waste acid liquid used in polysilicon texturing. Background technique [0002] During the texturing of polysilicon, a large amount of waste acid will be produced, including nitric acid, hydrofluoric acid and fluosilicic acid. At present, there are mainly five methods for the treatment of this waste mixed acid: neutralization method, evaporation process, direct incineration, membrane separation and resin adsorption technology. [0003] There are certain defects in the above five methods: [0004] One is the neutralization method, which not only needs to consume a large amount of alkaline substances, but also wastes the recyclable nitric acid and hydrofluoric acid in the waste acid. In addition, because the waste acid contains heavy metal ions, nit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/10C01B21/46C01B21/44C02F9/04C30B33/10C02F101/16C02F101/14
CPCC01B21/44C01B21/46C01B33/103C02F1/001C02F1/5236C02F1/66C02F9/00C02F2101/14C02F2101/16C02F2101/163C30B33/10
Inventor 蒋新赵会施利君
Owner SUZHOU KZONE EQUIP TECH
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