CN114853074B - NaFeF production by utilizing semiconductor waste acid 3 Is a method of (2) - Google Patents
NaFeF production by utilizing semiconductor waste acid 3 Is a method of (2) Download PDFInfo
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Abstract
The invention relates to a method for producing NaFeF by using semiconductor waste acid 3 The method of (1): 1) Adding excessive NaF into the semiconductor waste acid, reacting for 1-5 hours at 40-80 ℃, and carrying out solid-liquid separation after the reaction is finished to obtain filtrate 1 and solid slag 1; 2) Adding an iron oxide and a sodium compound into the filtrate 1, reacting for 1-24 hours at 10-100 ℃ under the stirring condition, and carrying out solid-liquid separation after the reaction is finished to obtain filtrate 2 and solid slag 2; 3) The solid slag 2 is obtained through calcination, separation and purification in the presence of a reducing agent. The method can recycle the semiconductor waste acid with high pollution, high risk and high concentration in the current electronic industry, and has the outstanding advantages of simple method, low cost, high product yield, high purity and the like.
Description
Technical Field
The invention belongs to the technical field of fluoride engineering, and particularly relates to a method for producing NaFeF by using semiconductor waste acid 3 Is a method of (2).
Background
The future power battery industry will be towards low cost, high safety, long life. Sodium ion batteries are used as one of power batteries, and because of the abundant storage of sodium salt raw materials, the sodium ion batteries have absolute price advantages compared with the most widely used lithium ion batteries at present. Sodium ion batteries are not new power batteries, and their development dates back to the eighties in the world, but have been slow due to limitations in electrode materials. Along with the situation of lithium resource shortage in the current lithium ion battery industry, the research and development of the sodium ion battery are also newly carried out, and more importance is paid.
NaFeF 3 Is an emerging sodium ion electrode material. Currently, naFeF is prepared 3 The method mainly prepares sodium hexafluoroferrite Na by an electrolytic method or a liquid phase deposition method 3 FeF 6 Then calcining to generate NaFeF 3 . For the intermediate product sodium hexafluoroferrite, the Chinese patent application CN201811067896.X adopts an electrolytic method to prepare sodium hexafluoroferrite, and the electrolytic method is simple in production method and high in reaction rate, but has high electrolytic cost and is difficult for large-scale industrial production. The Chinese patent application CN201710440651.6 adopts a liquid phase deposition method to prepare sodium hexafluoroferrite, and compared with an electrolytic method, the energy consumption is reduced, but the three wastes generated by the process flow are more, a reasonable solution is not provided for the treatment of waste residues and waste liquid, and the subsequent purification processing also increases the cost.
A large amount of waste acid liquid including nitric acid, fluosilicic acid and hydrofluoric acid is generated in the preparation process of the semiconductor, and if the waste acid liquid is directly discharged, the environment pollution and the waste of valuable components are caused, so that the waste acid liquid does not meet the environmental protection requirement. The conventional waste acid neutralization and dilution discharge can not fully utilize the effective components in the waste acid, so that waste is caused, secondary pollution is caused even if the waste acid is directly discharged after treatment, and therefore, the semiconductor waste acid is required to be treated more effectively.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for producing NaFeF by using semiconductor waste acid 3 The method can recycle the semiconductor waste acid with high pollution, high risk and high concentration in the current electronic industry, and has the outstanding advantages of simple method, low cost, high product yield, high purity and the like.
In order to achieve the above purpose, the invention adopts the following technical scheme:
NaFeF production by utilizing semiconductor waste acid 3 Comprising the steps of:
1) Adding excessive NaF into the semiconductor waste acid to react for 1-5 hours at the temperature of 10-40 ℃ so as to ensure that precipitation is complete, and carrying out solid-liquid separation after the reaction is finished to obtain filtrate 1 and solid slag 1;
2) Adding an iron oxide and a sodium compound into the filtrate 1, reacting for 1-10 hours at 10-40 ℃ under the condition of mechanical stirring, and carrying out solid-liquid separation after the reaction is finished to obtain filtrate 2 and solid slag 2 (for reducing HF loss, generally reacting at room temperature);
3) Calcining, separating and purifying the solid slag 2 in the presence of a reducing agent to obtain NaFeF 3 A solid.
Above-mentioned NaFeF production by using semiconductor waste acid 3 In the method, the semiconductor waste acid is waste acid generated in the semiconductor preparation process, mainly HNO 3 HF and H 2 SiF 6 A mixed solution is formed. HNO in semiconductor waste acid 3 The concentration is 5-30wt%, the concentration of HF is 10-25wt%, H 2 SiF 6 The concentration is 3-10wt%. In the step 1), the amount of NaF added is preferably 1.1 to 1.5 times the theoretical molar amount. NaF is providing Na + The method is used for precipitating fluosilicate ions, and simultaneously can react with nitric acid in the waste acid to generate sodium nitrate and hydrogen fluoride, so that a large amount of the fluoride ions in the waste acid system can be effectively and fully recycled.
Specifically, in step 1), the main component of the solid slag 1 is Na 2 SiF 6 Precipitating, heating to 350-450deg.C from room temperature under inert atmosphere, maintaining for 1-3 hr, heating to 550-650deg.C, and decomposing solid slag 1 to obtain SiF 4 Gas and NaF; naF can be used as a raw material to return to the step 1) for recycling, siF 4 After purification processing, the product is sold.
Further, in the step 2), the mechanical stirring speed is 200-1000 rpm, filtering is performed after the reaction is finished, and the filter residues are washed by deionized water and dried at 80-120 ℃ to obtain solid residue 2. The main component of the solid slag 2 is Na 3 FeF 6 。
Further preferably, in step 2), the iron oxide is iron oxide, iron oxyhydroxide, or the like.
Further preferably, in step 2), the sodium compound may be one or more of sodium hydroxide, sodium carbonate, sodium bicarbonate, sodium acetate, and the like.
Further, in step 2), the molar ratio of the F element in the filtrate 1 to the Fe element in the iron oxide and the Na element in the sodium compound is 6:1:2 to 3.
Specifically, in step 3), the reducing agent is H 2 CO, C, or the like, preferably H 2 。
Specifically, in the step 3), the calcination temperature is 800-1200 ℃ and the calcination time is 2-24 h.
Further, in step 2), the main component in the filtrate 2 is NaNO 3 Cooling, crystallizing, purifying, and selling; in the step 3), the solid slag 2 is calcined and heated for reduction decomposition, and the generated byproducts NaF and HF are returned to the step 1) to be recycled as raw materials.
The main reaction equations involved in the method of the invention are as follows:
H 2 SiF 6 +2NaF→Na 2 SiF 6 ↓+2HF
HNO 3 +NaF→NaNO 3 +HF
Na 2 SiF 6 →2NaF+SiF 4 ↑
6NaOH+12HF+Fe 2 O 3 →2Na 3 FeF 6 +9H 2 O
2Na 3 FeF 6 +H 2 →4NaF+2NaFeF 3 +2HF↑
compared with the prior art, the method has the following beneficial effects:
compared with the traditional semiconductor waste acid recovery process, the process generates hydrofluoric acid while preferentially utilizing the hydrofluoric acid in the waste liquid, fully recovers and utilizes valuable fluorine components, meets the environmental protection requirement, has simple process flow and is suitable for large-scale production.
Drawings
FIG. 1 is a process flow diagram of the method of the present invention.
Detailed Description
The following describes the technical scheme of the present invention in further detail with reference to examples, but the scope of the present invention is not limited thereto.
In the examples below, the starting materials are all commercially available products which are commercially available as they are. Room temperature refers to 25±5 ℃.
The semiconductor waste acid is waste acid generated in the semiconductor preparation process of a certain factory, mainly HNO 3 HF and H 2 SiF 6 A mixed solution is formed.
Example 1
NaFeF production by utilizing semiconductor waste acid 3 The method comprises the following steps:
1) 100kg of the mixture contains 5% HNO by mass 3 、10%HF、3% H 2 SiF 6 Adding 7.62kg of NaF into the waste acid liquid generated in the semiconductor preparation process to react, controlling the reaction temperature to 40 ℃ and the reaction time to 1h, and filtering after the reaction is finished to obtain filtrate 1 and solid slag 1;
2) Adding 11.18kg sodium hydroxide and 9.04kg ferric oxide into the filtrate 1, reacting at 40deg.C under stirring for 1 hr, filtering to obtain filtrate 2 and residue, washing the residue with deionized water, and drying at 120deg.C to obtain 26.6kg solid residue 2 (Na 3 FeF 6 ）；
3) 26.60kg of solid slag 2 (Na 3 FeF 6 ) At H 2 Reducing and calcining for 2h at 1200 ℃ under atmosphere, washing with water, filtering and drying to obtain 14.78kg NaFeF 3 The yield can reach 96.23 percent, and the purity can reach 99.17 percent.
The main component of the solid slag 1 in the step 1) is Na 2 SiF 6 Precipitating, heating to 400 ℃ from room temperature under inert atmosphere, preserving heat for 2h, and then heating to 600 ℃ to decompose solid slag 1 to obtain SiF 4 Gas and NaF; naF can be used as a raw material to return to the step 1) for recycling, siF 4 After purification processing, the product is sold. In step 2), the main component in the filtrate 2 is NaNO 3 Cooling, crystallizing, purifying, and selling; in the step 3), byproducts NaF and HF generated by the calcination of the solid slag 2 can be returned to the step 1) to be recycled as raw materials.
Example 2
Utilizing semiconductor wasteAcid production of NaFeF 3 The method comprises the following steps:
1) 100kg of the mixture contains 15% HNO by mass 3 、17%HF、7% H 2 SiF 6 Adding 18.31kg of NaF into the waste acid liquid generated in the preparation process of the semiconductor to react, controlling the reaction temperature to 25 ℃, and filtering after the reaction is finished to obtain filtrate 1 and solid slag 1, wherein the reaction time is 3 hours;
2) Adding 28.73kg sodium carbonate and 17.12kg ferric oxide into the filtrate 1, controlling the reaction temperature to be 30 ℃, stirring and reacting for 5 hours, filtering after the reaction is finished to obtain filtrate 2 and filter residues, washing the filter residues by deionized water, and drying the filter residues at 100 ℃ to obtain 50.38kg solid residue 2 (Na 3 FeF 6 ）；
3) 50.38kg of solid slag 2 (Na 3 FeF 6 ) At H 2 Reducing and calcining for 12h at 1000 ℃ under atmosphere, washing with water, filtering and drying to obtain 28.18kg NaFeF 3 The yield is 96.82%, and the purity can reach 99.24%.
Example 3
NaFeF production by utilizing semiconductor waste acid 3 The method comprises the following steps:
1) 100kg of the mixture contains 30% HNO by mass 3 、25%HF、10% H 2 SiF 6 Adding 28.42kg of NaF into the waste acid liquid generated in the preparation process of the semiconductor to react, controlling the reaction temperature to be 10 ℃, and filtering after the reaction is finished for 5 hours to obtain filtrate 1 and solid slag 1;
2) Adding 75.20kg sodium acetate and 28.57kg ferric hydroxide into the filtrate 1, reacting at 10deg.C under stirring for 10 hr, filtering to obtain filtrate 2 and residue, washing the residue with deionized water, and drying at 80deg.C to obtain 75.32kg solid residue 2 (Na 3 FeF 6 ）；
3) 75.32kg of solid slag 2 (Na 3 FeF 6 ) At H 2 Reducing and calcining for 24 hours at 800 ℃ under atmosphere, washing with water, filtering and drying to obtain 42.13kg NaFeF 3 The yield can reach 96.53 percent, and the purity can reach 99.31 percent.
Claims (7)
1. Utilize halfNaFeF production by conductor waste acid 3 Is characterized by comprising the following steps:
1) Adding excessive NaF into the semiconductor waste acid, reacting for 1-5 hours at the temperature of 10-40 ℃, and carrying out solid-liquid separation after the reaction is finished to obtain filtrate 1 and solid slag 1;
2) Adding an iron oxide and a sodium compound into the filtrate 1, reacting for 1-10 hours at 10-40 ℃ under the stirring condition, and carrying out solid-liquid separation after the reaction is finished to obtain filtrate 2 and solid slag 2;
3) Calcining, separating and purifying the solid slag 2 in the presence of a reducing agent to obtain the solid slag;
the semiconductor waste acid is waste acid generated in the semiconductor preparation process; HNO in semiconductor waste acid 3 The concentration is 5-30wt%, the concentration of HF is 10-25wt%, H 2 SiF 6 The concentration is 3-10wt%;
in the step 2), the iron oxide is ferric oxide or ferric hydroxide;
in the step 2), the sodium compound is one or more than two of sodium hydroxide, sodium carbonate, sodium bicarbonate and sodium acetate.
2. The method for producing NaFeF by using semiconductor waste acid according to claim 1 3 The method is characterized in that in the step 1), the main component of the solid slag 1 is Na 2 SiF 6 Precipitating, heating to 350-450deg.C from room temperature under inert atmosphere, maintaining for 1-3 hr, heating to 550-650deg.C, and decomposing solid residue 1 to obtain SiF 4 Gas and NaF; returning NaF as raw material to step 1) for recycling, siF 4 After purification processing, the product is sold.
3. The method for producing NaFeF by using semiconductor waste acid according to claim 1 3 The method is characterized in that in the step 2), filtering is carried out after the reaction is finished, and filter residues are dried at 80-120 ℃ after being washed by deionized water, so as to obtain solid residues 2.
4. The method for producing NaFeF by using semiconductor waste acid according to claim 1 3 In the step 2), F element in the filtrate 1, fe element in the iron oxide and sodiumThe molar ratio of Na element in the compound is 6:1:2 to 3.
5. The method for producing NaFeF by using semiconductor waste acid according to claim 1 3 Characterized in that in step 3), the reducing agent is H 2 CO, or C.
6. The method for producing NaFeF by using semiconductor waste acid according to claim 5 3 The method is characterized in that in the step 3), the calcination temperature is 800-1200 ℃ and the calcination time is 2-24 h.
7. The method for producing NaFeF by using semiconductor waste acid according to claim 1 3 Is characterized in that in the step 2), the main component of the filtrate 2 is NaNO 3 Cooling, crystallizing, purifying, and selling; in the step 3), byproducts NaF and HF generated by calcining the solid slag 2 are returned to the step 1) to be recycled as raw materials.
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| JP5721171B2 (en) * | 2011-02-21 | 2015-05-20 | 国立大学法人九州大学 | Electrode active material and method for producing the same |
| CN107104248B (en) * | 2016-02-22 | 2019-06-11 | 中国科学院上海硅酸盐研究所 | A kind of potassium/sodium-ion battery is with opening frame fluoride positive electrode and preparation method thereof |
| CN107293712A (en) * | 2017-06-12 | 2017-10-24 | 湖南工程学院 | A kind of preparation method for being applied to sodium or anode material for lithium-ion batteries hexafluoro sodium ferrite and its covering material |
| CN109252181B (en) * | 2018-09-13 | 2020-09-01 | 湖南工程学院 | Method for preparing sodium hexafluoroferrite by electrolysis |
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