CN115283422B - Treatment method of glass etching waste residues - Google Patents
Treatment method of glass etching waste residues Download PDFInfo
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- CN115283422B CN115283422B CN202210860676.2A CN202210860676A CN115283422B CN 115283422 B CN115283422 B CN 115283422B CN 202210860676 A CN202210860676 A CN 202210860676A CN 115283422 B CN115283422 B CN 115283422B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/70—Chemical treatment, e.g. pH adjustment or oxidation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/40—Destroying solid waste or transforming solid waste into something useful or harmless involving thermal treatment, e.g. evaporation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
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Abstract
The invention discloses a method for treating glass etching waste residues, which comprises the steps of adding waste acid into a glass etching waste residue dissolution and neutralization reaction system, increasing the temperature of the reaction system by utilizing the dilution heat and the neutralization reaction heat of the waste acid, and accelerating the dissolution reaction of the glass etching waste residues through heating. The method can obviously improve the dissolution rate of the glass etching waste residues, does not need an external heat source, is simple and energy-saving, can synchronously treat high-concentration waste acid, and greatly improves the production efficiency.
Description
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a method for treating glass etching waste residues.
Background
With the development of modern technology, electronic display devices are being thinned, and the thickness of display glass is reduced to below 0.3 mm. Ultrathin glass is difficult to manufacture directly, and is usually subjected to thinning treatment. Acid treatment is the most commonly used surface thinning treatment, i.e. using hydrofluoric acid (HF) and ammonium bifluoride (NH) 4 HF 2 ) And (3) performing etching thinning treatment by using mixed acid as a main component. In the acid treatment, hydrofluoric acid reacts with the glass to peel off the surface of the glass layer by layer. But the etching process can form substances such as silicon dioxide, fluorosilicate and the like which are insoluble in water to be separated out, and a large amount of etching waste residues are generated after the solid-liquid separation of etching waste liquid, thus the etching waste liquid belongs to dangerous waste, and the code HW32 is required to be treated by a hazardous waste disposal qualification unit.
In recent years, with the rapid development of industries such as TFT-LCD in China, new glass thinning factories are increasingly built, waste residues generated by etching are greatly increased, and the treatment of the waste residues becomes a serious problem. The main treatment method in the industry at present is a lime neutralization treatment method, which utilizes excessive lime emulsion to react with glass etching waste residues, neutralizes acid components in the waste residues and converts fluorine into calcium fluoride (CaF) 2 ) And (3) carrying out solid-liquid separation on the sediment, and then carrying out landfill or recycling treatment. However, in the treatment process, the dissolution reaction speed of the glass etching waste residues in the lime milk is low, and the stirring time is usually more than 3 hours to meet the solid-liquid separation feeding condition, so that the limit is extremely largeThe throughput to handle it is made. Meanwhile, for a general hazardous waste disposal unit, high-concentration waste acid (hazardous waste code HW 34) can be treated, and in order to avoid over-high-temperature bumping overflow in the treatment process of the waste acid, the high-concentration waste acid needs to be diluted and cooled and then undergoes a neutralization reaction, and the process is time-consuming and does not well utilize heat energy released by dilution.
In summary, the existing glass etching waste residue treatment has the problems of low efficiency and difficulty in meeting the requirements of productivity.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a treatment method for improving the treatment efficiency of glass etching waste residues.
The aim of the invention can be achieved by the following technical scheme:
a method for treating glass etching waste residues comprises the following steps:
(1) Mixing glass etching waste residues with lime milk to carry out dissolution and neutralization reaction;
(2) Adding a certain amount of waste acid into the reaction system in the step (1), and fully stirring for reaction to quickly raise the temperature of the system to a certain temperature so as to completely dissolve the glass etching waste residues;
(3) After the glass etching waste residues are completely dissolved, carrying out solid-liquid separation to obtain dehydrated sludge and filtrate;
(4) Further processing the dehydrated sludge and filtrate obtained in the step (3);
further, the glass etching waste residue contains H 2 SiF 6 、NH 4 HF 2 、HF、HNO 3 、H 2 SO 4 Fluorosilicates, siO 2 And water; further, the glass etching waste residue contains 1 to 15 percent of H by mass concentration 2 SiF 6 、1％～10％NH 4 HF 2 、5％～20％HF、1％～5％HNO 3 、1％～5％H 2 SO 4 5 to 25 percent of fluorosilicate and 10 to 75 percent of SiO 2 And water;
further, in the step (1), the mass concentration of lime milk is 1% -30%;
further, in the step (1), the mass ratio of the lime milk to the glass etching waste residue is 1-100: 1, a step of; further, in the step (1), the mass ratio of the lime milk to the glass etching waste residue is 1-20: 1, a step of;
further, in the step (2), the waste acid at least contains any two of hydrofluoric acid, sulfuric acid, hydrochloric acid, nitric acid and phosphoric acid, and H in the waste acid + The concentration of (2) is 0.001 mol/L-30 mol/L;
further, in the step (2), the mass ratio of the waste acid to the glass etching waste residue is 0.01-100: 1, a step of; further, in the step (2), the mass ratio of the waste acid to the glass etching waste residue is 0.1-50: 1, a step of; further, in the step (2), the mass ratio of the waste acid to the glass etching waste residue is 0.1-10: 1, a step of;
further, in the step (2), the temperature of the system is rapidly increased to 30-100 ℃;
further, in the step (2), the stirring mode is selected from any one or more of mechanical stirring, liquid reflux stirring or gas stirring;
further, in the step (2), the time of complete dissolution is 60-240 min; further, the dissolution time is 80-220 min; further, the dissolution time is 100-160 min;
further, in the step (3), the solid-liquid separation method is selected from filter pressing, suction filtration or filtration after centrifugation;
further, in the step (4), the dehydrated sludge is treated by landfill or other recycling treatment modes;
further, in the step (4), the filtrate is continuously used for preparing lime milk or is treated by other conventional methods.
Advantageous effects
The invention utilizes the heat released by the dilution and neutralization reaction of waste acid to raise the temperature of the system, and the temperature rise can obviously improve the dissolution rate of glass etching waste residues in lime milk, thereby effectively improving the production efficiency.
Compared with the prior art, the invention has the following advantages:
1. the process method is simple and the process efficiency is high. The glass etching residues are solid acidic mixtures, the dissolution time of which can be considered to be equivalent to the neutralization reaction time, but under general treatment conditions, the dissolution time is long because the silicon dioxide hydrate in the residues is wrapped and cannot be effectively crushed. The patent utilizes the dilution heat and the neutralization reaction heat of the waste acid to improve the dissolution temperature and quicken the dissolution of the waste residue, thereby improving the reaction speed. The neutralization reaction of waste acid and lime milk and the heat released by dilution are utilized to raise the temperature of a reaction system, so that the dissolution reaction rate of glass etching waste residues is obviously improved, the reaction time is shortened, and the heat energy is saved;
2. the lime adding amount needs to meet the requirement that the lime adding amount is an acidic mixture of liquid and solid state with glass etching waste residues and sulfuric acid, and the waste acid and the glass etching waste residues are typical treatment objects of a hazardous waste treatment unit physical and chemical treatment unit, so that the waste acid is easy to obtain.
Detailed Description
The specific implementation process comprises the following steps of: the lime addition amount needs to meet the requirement of neutralization reaction with glass etching waste residues and sulfuric acid, the final pH value is neutral 6-9, the waste acid addition amount is used for increasing the temperature of a reaction system to a specified temperature, and the heat for temperature increase is derived from dilution heat and neutralization reaction heat of the waste acid. Neutralization heat is according to H + And OH (OH) - The exothermic heat of reaction is calculated to be 57.4kJ/mol, and the temperature rise can be calculated approximately as the temperature rise of water in the system.
The invention is further illustrated by the following examples. The embodiment is implemented on the premise of the technical scheme of the invention, and a detailed implementation mode and a specific operation flow are provided, but the protection scope of the invention is not limited to the following embodiment.
Comparative example 1
Adding 3.3 times of glass etching waste residues into the beakers 1, 2, 3, 4 and 5 respectively, wherein the concentration is 15wt%; 2.5 times of the weight and the concentration is 20 weight percent; lime milk with the mass of 2 times and the concentration of 25 percent; lime milk with the mass of 3.8 times and the concentration of 20 percent; lime milk with the mass of 3.53 times and the concentration of 20 percent. Mechanically stirring at 25deg.C at room temperature, and dissolving for 275min, 308min, 350min, 320min, and 330min.
Example 1
A method for treating glass etching waste residues comprises the following steps:
(1) Adding glass etching waste residues into lime milk, mixing, dissolving and neutralizing, wherein the glass etching waste residues are prepared from 1% -15% of H 2 SiF 6 、1％～10％NH 4 HF 2 、5％～20％HF、1％～5％HNO 3 、1％～5％H 2 SO 4 5 to 25 percent of fluorosilicate and 10 to 75 percent of SiO 2 And water, wherein the mass ratio of the lime milk to the glass etching waste residue is 4.7:1, lime milk mass concentration is 15%; (2) Adding a certain amount of waste acid into the reaction system in the step (1), wherein the waste acid contains hydrofluoric acid, sulfuric acid and hydrochloric acid, and H in the waste acid + The concentration of (2) is 15.3mol/L; the mass ratio of the waste acid to the glass etching waste residue is 0.4:1, a step of; fully stirring in a mechanical stirring mode to quickly raise the temperature of the system to 42 ℃ so as to completely dissolve the glass etching waste residues, wherein the complete dissolution time is 220min, and the dissolution time is accelerated by 20%; (3) After the glass etching waste residues are completely dissolved, carrying out solid-liquid separation in a suction filtration mode to obtain dehydrated sludge and filtrate; (4) And (3) further treating the dehydrated sludge and filtrate obtained in the step (3), wherein the dehydrated sludge is buried, and the filtrate is continuously used for preparing lime milk.
Example 2
A method for treating glass etching waste residues comprises the following steps:
(1) Adding glass etching waste residues into lime milk, mixing, dissolving and neutralizing, wherein the glass etching waste residues are prepared from 1% -15% of H 2 SiF 6 、1％～10％NH 4 HF 2 、5％～20％HF、1％～5％HNO 3 、1％～5％H 2 SO 4 、5％～25% fluorosilicate and 10% -75% SiO 2 And water, wherein the mass ratio of the lime milk to the glass etching waste residue is 8.1:1, lime milk mass concentration is 15%; (2) Adding a certain amount of waste acid into the reaction system in the step (1), wherein the waste acid contains sulfuric acid, hydrochloric acid, nitric acid and phosphoric acid, and H in the waste acid + The concentration of (2) is 25.1mol/L; the mass ratio of the waste acid to the glass etching waste residue is 1:1, a step of; fully stirring in a gas stirring mode to quickly raise the temperature of the system to 79 ℃ to completely dissolve the glass etching waste residues, wherein the complete dissolution time is 80min, and the dissolution time is increased by 70.1%; (3) After the glass etching waste residues are completely dissolved, carrying out solid-liquid separation by adopting a centrifugal filtration mode to obtain dehydrated sludge and filtrate; (4) And (3) further treating the dehydrated sludge and filtrate obtained in the step (3), wherein the dehydrated sludge is buried, and the filtrate is continuously used for preparing lime milk.
Example 3
A method for treating glass etching waste residues comprises the following steps:
(1) Adding glass etching waste residues into lime milk, mixing, dissolving and neutralizing, wherein the glass etching waste residues are prepared from 1% -15% of H 2 SiF 6 、1％～10％NH 4 HF 2 、5％～20％HF、1％～5％HNO 3 、1％～5％H 2 SO 4 5 to 25 percent of fluorosilicate and 10 to 75 percent of SiO 2 And water, wherein the mass ratio of the lime milk to the glass etching waste residue is 8.1:1, lime milk mass concentration is 15%; (2) Adding a certain amount of waste acid into the reaction system in the step (1), wherein the waste acid contains sulfuric acid, hydrofluoric acid, nitric acid and phosphoric acid, and H in the waste acid + The concentration of (2) is 30mol/L; the mass ratio of the waste acid to the glass etching waste residue is 0.8:1, a step of; fully stirring in a mechanical stirring mode to quickly raise the temperature of the system to 79 ℃ to completely dissolve the glass etching waste residues, wherein the complete dissolution time is 120min, and the dissolution time is increased by 63.2%; (3) After the glass etching waste residues are completely dissolved, carrying out solid-liquid separation in a suction filtration mode to obtain dehydrated sludge and filtrate; (4) Further processing the dehydrated sludge and filtrate obtained in the step (3), wherein the dehydrated sludge adoptsLandfill is carried out, and the filtrate is continuously used for preparing lime milk.
Example 4
A method for treating glass etching waste residues comprises the following steps:
(1) Adding glass etching waste residues into lime milk, mixing, dissolving and neutralizing, wherein the glass etching waste residues are prepared from 1% -15% of H 2 SiF 6 、1％～10％NH 4 HF 2 、5％～20％HF、1％～5％HNO 3 、1％～5％H 2 SO 4 5 to 25 percent of fluorosilicate and 10 to 75 percent of SiO 2 And water, wherein the mass ratio of the lime milk to the glass etching waste residue is 3.8:1, lime milk mass concentration is 20%; (2) Adding a certain amount of waste acid into the reaction system in the step (1), wherein the waste acid contains hydrofluoric acid, nitric acid and phosphoric acid, and H in the waste acid + The concentration of (2) is 24.4mol/L; the mass ratio of the waste acid to the glass etching waste residue is 0.33:1, a step of; fully stirring in a gas stirring mode to quickly raise the temperature of the system to 60 ℃ so as to completely dissolve the glass etching waste residues, wherein the complete dissolution time is 120min, and the dissolution time is increased by 64.1%; (3) After the glass etching waste residues are completely dissolved, carrying out solid-liquid separation in a suction filtration mode to obtain dehydrated sludge and filtrate; (4) And (3) further treating the dehydrated sludge and filtrate obtained in the step (3), wherein the dehydrated sludge is buried, and the filtrate is continuously used for preparing lime milk.
Example 5
A method for treating glass etching waste residues comprises the following steps:
(1) Adding glass etching waste residues into lime milk, mixing, dissolving and neutralizing, wherein the glass etching waste residues are prepared from 1% -15% of H 2 SiF 6 、1％～10％NH 4 HF 2 、5％～20％HF、1％～5％HNO 3 、1％～5％H 2 SO 4 5 to 25 percent of fluorosilicate and 10 to 75 percent of SiO 2 And water, wherein the mass ratio of the lime milk to the glass etching waste residue is 3.53:1, lime milk mass concentration is 20%; (2) Adding a certain amount of waste acid into the reaction system in the step (1), wherein the waste acid containsSulfuric acid, hydrofluoric acid, nitric acid, phosphoric acid, H in waste acid + The concentration of (2) is 14.9mol/L; the mass ratio of the waste acid to the glass etching waste residue is 0.41:1, a step of; fully stirring in a liquid reflux stirring mode to quickly raise the temperature of the system to 60 ℃ so as to completely dissolve the glass etching waste residues, wherein the complete dissolution time is 120min, and the dissolution time is accelerated by 62.5%; (3) After the glass etching waste residues are completely dissolved, performing solid-liquid separation in a filter pressing mode to obtain dehydrated sludge and filtrate; (4) And (3) further treating the dehydrated sludge and filtrate obtained in the step (3), wherein the dehydrated sludge is buried, and the filtrate is continuously used for preparing lime milk.
Claims (5)
1. The method for treating the glass etching waste residues is characterized by comprising the following steps:
(1) Mixing glass etching waste residues and lime milk for dissolution and neutralization reaction, wherein the mass ratio of the lime milk to the glass etching waste residues is 1-100: 1, the glass etching waste residue contains 1% -15% of H2SiF6, 1% -10% of NH4HF2, 5% -20% of HF, 1% -5% of HNO3, 1% -5% of H2SO4, 5% -25% of fluorosilicate, 10% -75% of SiO2 and water, wherein the mass concentration of lime milk is 1% -30%;
(2) Adding a certain amount of waste acid into the reaction system in the step (1), and fully stirring for reaction to quickly raise the temperature of the system to 30-100 ℃ so as to completely dissolve the glass etching waste residues for 60-240 min, wherein the mass ratio of the waste acid to the glass etching waste residues is 0.01-100: 1, a step of; the waste acid at least contains any two of hydrofluoric acid, sulfuric acid, hydrochloric acid, nitric acid and phosphoric acid, the concentration of H+ in the waste acid is 0.001 mol/L-30 mol/L, and the stirring mode is selected from any one or more of mechanical stirring, liquid reflux stirring or gas stirring;
(3) After the glass etching waste residues are completely dissolved, carrying out solid-liquid separation to obtain dehydrated sludge and filtrate, wherein the solid-liquid separation method is selected from filter pressing, suction filtration or centrifugal filtration;
(4) Further processing the dehydrated sludge and filtrate obtained in the step (3), wherein the dehydrated sludge is processed by landfill or other recycling processing modes, and the filtrate is continuously used for preparing lime milk.
2. The method for treating glass etching residues according to claim 1, wherein in the step (1), the mass ratio of the lime milk to the glass etching residues is 1-20: 1.
3. the method for treating glass etching residues according to claim 1, wherein in the step (2), the mass ratio of waste acid to glass etching residues is 0.1-50: 1.
4. the method for treating glass etching residues according to claim 1, wherein in the step (2), the mass ratio of waste acid to glass etching residues is 0.1-10: 1.
5. the method for treating glass etching residues according to claim 1, wherein in the step (2), the time for complete dissolution is 100-160 min.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210860676.2A CN115283422B (en) | 2022-07-21 | 2022-07-21 | Treatment method of glass etching waste residues |
| PCT/CN2023/107190 WO2024017129A1 (en) | 2022-07-21 | 2023-07-13 | Method for treating waste residues from glass etching |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210860676.2A CN115283422B (en) | 2022-07-21 | 2022-07-21 | Treatment method of glass etching waste residues |
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| CN115283422A CN115283422A (en) | 2022-11-04 |
| CN115283422B true CN115283422B (en) | 2023-10-31 |
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| WO (1) | WO2024017129A1 (en) |
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| CN115283422B (en) * | 2022-07-21 | 2023-10-31 | 上海市政工程设计研究总院（集团）有限公司 | Treatment method of glass etching waste residues |
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| WO2024017129A1 (en) | 2024-01-25 |
| CN115283422A (en) | 2022-11-04 |
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