CN114965326B - Method for measuring nickel content in waste residue generated by nitrogen trifluoride electrolysis - Google Patents
Method for measuring nickel content in waste residue generated by nitrogen trifluoride electrolysis Download PDFInfo
- Publication number
- CN114965326B CN114965326B CN202210897749.5A CN202210897749A CN114965326B CN 114965326 B CN114965326 B CN 114965326B CN 202210897749 A CN202210897749 A CN 202210897749A CN 114965326 B CN114965326 B CN 114965326B
- Authority
- CN
- China
- Prior art keywords
- slag
- nickel content
- nickel
- soluble
- nitrogen trifluoride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to the technical field of determination of metal content in electrolytic waste residues, in particular to a method for determining nickel content in waste residues generated by nitrogen trifluoride electrolysis. The method for measuring the content of nickel in waste residue generated in nitrogen trifluoride electrolysis comprises the following steps: firstly, distinguishing soluble slag and insoluble slag from waste residues generated in nitrogen trifluoride electrolysis, then respectively measuring the nickel content in the soluble slag and the nickel content in the insoluble slag, and finally calculating the nickel content in the waste residues generated in nitrogen trifluoride electrolysis according to the nickel content in the soluble slag and the nickel content in the insoluble slag. The invention provides a method for measuring the content of nickel in waste residue generated by nitrogen trifluoride electrolysis, which has the advantages of simple operation steps, high accuracy, high efficiency and high utilization value.
Description
Technical Field
The invention relates to the technical field of determination of metal content in electrolytic waste residues, in particular to a method for determining nickel content in waste residues generated by nitrogen trifluoride electrolysis.
Background
The nickel has high hardness, good toughness, iron magnetism, good polishing performance and strong corrosion resistance, thereby being widely applied in the industries of aerospace, nuclear engineering, energy power, transportation and the like. Because of the different nickel content in the electrolytic waste residue, the price fluctuation is larger, so the market liquidity of the nickel-containing waste residue is stronger.
During the electrolysis of nitrogen trifluoride, nickel is gradually dissolved and corroded by the electrolyte, and part of nickel in the electrolyte is plated out at a cathode, and the other part of nickel is accumulated at the bottom of an electrolytic tank in the form of salt or a complex, thereby influencing the electrolysis efficiency. The deposits at the bottom of the cell must be cleaned, which increases the production costs. The main components of the waste residue after cleaning are nickel, iron, copper and other metal simple substances or metal fluorides, and doped ammonium bifluoride and other substances. The recycling value is different due to different nickel content in the waste residue. The nickel content in the waste residue determines the market price, so that the quantitative determination of the nickel content in the waste residue is particularly important. In the prior art, more qualitative test methods are used, but the quantitative determination of the nickel content in the waste residue is rare. Because the components of the waste residue are complex, a complex reagent is required to be added for measuring the nickel content, and the production application is not facilitated. Therefore, the quantitative determination of the nickel content in the waste residue is a bottleneck difficult to break through in production.
CN105004682A discloses a detection reagent for nickel ions in water and a detection method thereof, wherein a detection reagent A boric acid, potassium chloride, sodium hydroxide, an oxidant, a masking agent, dimethylglyoxime, N-diethyl-p-phenylenediamine, sulfanilic acid, a reagent B sodium hydroxide, a masking agent and dimethylglyoxime are adopted, and then detection is carried out.
CN103969259A discloses a method for detecting nickel ions in water after primary pretreatment of electroplating wastewater, eight standard reagents are prepared, and the method is used for limited measurement, and has the disadvantages of complicated steps, multiple reagent types, short storage time of detection reagents and no contribution to production and wide application in quantitative determination.
CN108918512B discloses a detection reagent for stainless steel nickel content and a detection method for stainless steel nickel content, which adopt reagents of dimethylglyoxime, ammonium persulfate, chitosan, barium sulfate, sodium hydroxide, disodium ethylene diamine tetraacetate, cationic guar gum, methylene bisacrylamide and potassium sodium tartrate. Although the detection method is simple and effective, the detection method is not suitable for the complex reagent with larger alkalinity in the electrolytic waste residue.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for measuring the content of nickel in waste residues generated by nitrogen trifluoride electrolysis, which has the advantages of simple operation steps, high accuracy, high efficiency and high utilization value.
The invention relates to a method for measuring nickel content in waste residue generated by nitrogen trifluoride electrolysis, which comprises the following steps: firstly, distinguishing soluble slag and insoluble slag from waste residues generated by nitrogen trifluoride electrolysis, then respectively measuring the nickel content in the soluble slag and the nickel content in the insoluble slag, and finally calculating the nickel content in the waste residues generated by nitrogen trifluoride electrolysis according to the nickel content in the soluble slag and the nickel content in the insoluble slag.
Preferably, the step of distinguishing soluble slag from insoluble slag of the waste slag generated in the nitrogen trifluoride electrolysis comprises the following steps: dissolving the waste residue in water according to the mass ratio of 1:2-1:3, and performing pressure filtration on the waste residue with a 200-mesh sieve to obtain solid which is insoluble residue; and introducing ammonia gas into the filtrate until no precipitate is generated, and centrifuging at 2000-2500 r/min until no water is generated, wherein the obtained solid is soluble slag. . The filter pressing adopts a plate-and-frame filter press. The centrifugation is performed by a centrifuge.
The refractory slag contains: iron oxide, nickel oxide, copper oxide, iron fluoride, ammonium fluoride, copper fluoride, nickel fluoride, and a metal simple substance. The soluble slag comprises: iron fluoride, ammonium fluoride, copper fluoride, ammonium nickel fluoride, ammonium ferric compounds, ammonium fluoride, and the like. The main factor for separating insoluble slag and soluble slag is the difference of the solubility of fluoride, metal simple substance and metal oxide in the slag in water and alkaline environment.
The method for measuring the nickel content in the waste residue generated by nitrogen trifluoride electrolysis comprises the following steps of:
a1, accurately weighing and calcining soluble slag, keeping the temperature of the soluble slag at 240-280 ℃, continuously calcining for 5-8h, and stirring once every 15-20min in the process;
b1, accurately weighing the calcined soluble slag, adding water, adding a nitric acid solution for dissolving, heating to 80-90 ℃, reacting for 6-8h, adding water into a beaker in the process, and maintaining the liquid level at the position before heating;
and c1, performing suction filtration after the reaction is finished, weighing the volume of the filtrate, measuring the mass concentration of the nickel in the filtrate by using an atomic absorption method, and calculating to obtain the nickel content in the soluble slag.
The atomic absorption method is based on the method for measuring the atomic absorption spectrum of the metal elements in the SY/T5161-2002 rock.
Preferably, the residual quantity of the soluble slag after calcination in the step a1 is 36-40% of the mass before calcination, and the color is brick red.
Preferably, the mass ratio of the soluble slag calcined in the step b1 to the nitric acid is 1.
The method for measuring the nickel content in the waste residue generated by nitrogen trifluoride electrolysis comprises the following steps of:
a2, accurately weighing and calcining the insoluble slag, keeping the temperature of the insoluble slag at 240-280 ℃, continuously calcining for 7-9h, and stirring once every 15-20min in the process;
b2, accurately weighing the calcined insoluble slag, adding water, adding a nitric acid solution for dissolving, heating to 80-90 ℃, reacting for 6-8h, adding water into the beaker in the process, and maintaining the liquid level at the position before heating;
and c2, performing suction filtration after the reaction is finished, weighing the volume of the filtrate, measuring the mass concentration of the nickel in the filtrate by using an atomic absorption method, and calculating to obtain the nickel content in the refractory slag.
Preferably, the residual quantity of refractory slag after calcination in the step a2 is 80-90% of the mass before calcination, and the color is brick red.
Preferably, the mass ratio of the refractory slag calcined in the step b2 to the nitric acid is 1.
Preferably, the calculation formula of the nickel content in the soluble slag is as follows:
preferably, the calculation formula of the nickel content in the refractory slag is as follows:
specifically, the method for measuring the content of nickel in waste residues generated by nitrogen trifluoride electrolysis comprises the following steps:
(1) Firstly, distinguishing soluble slag and insoluble slag from waste slag generated by nitrogen trifluoride electrolysis: dissolving the waste residue in water according to the mass ratio of 1:2-1:3, and performing pressure filtration on the waste residue with 200 meshes to obtain solid which is refractory residue; introducing ammonia gas into the filtrate until no precipitate is generated, centrifuging at 2000r/min-2500r/min until no water is generated, and obtaining solid which is soluble slag;
(2) Determining the nickel content in the soluble slag:
a1, accurately weighing and calcining soluble slag, keeping the temperature of the soluble slag at 240-280 ℃, continuously calcining for 5-8h, stirring every 15-20min in the process, wherein the residual amount of the soluble slag after calcination is 36-40% of the mass before calcination, and the color is brick red;
b1, accurately weighing the calcined soluble slag, adding water, adding a nitric acid solution for dissolution, heating the calcined soluble slag to 80-90 ℃ for reaction for 6-8h, wherein the mass ratio of the calcined soluble slag to the nitric acid is 1-10.5;
c1, performing suction filtration after the reaction is finished, weighing the volume of the filtrate, measuring the mass concentration of nickel in the filtrate by using an atomic absorption method, and calculating to obtain the nickel content in the soluble slag;
(3) Determining the nickel content in the refractory slag:
a2, accurately weighing and calcining the refractory slag, keeping the temperature of the refractory slag at 240-280 ℃, continuously calcining for 7-9h, stirring once every 15-20min in the process, wherein the residual amount of the refractory slag after calcination is about 80-90% of that before calcination, and the color of the refractory slag is brick red;
b2, accurately weighing the calcined insoluble slag, adding water, adding a nitric acid solution for dissolution, heating the calcined insoluble slag to 80-90 ℃ for reaction for 6-8h, wherein the mass ratio of the calcined insoluble slag to the nitric acid is 1;
c2, performing suction filtration after the reaction is finished, weighing the volume of the filtrate, measuring the mass concentration of nickel in the filtrate by using an atomic absorption method, and calculating to obtain the nickel content in the refractory slag;
(4) And (3) calculating the total content of nickel in waste residues generated by nitrogen trifluoride electrolysis, wherein the calculation formula is as follows:
the method for measuring the nickel content in the waste residue generated by nitrogen trifluoride electrolysis firstly distinguishes the waste residue from the insoluble residue, and has influence on the measurement of the nickel content due to different solubilities of other substances in the soluble residue and the insoluble residue, then respectively measures the nickel content in the soluble residue and the insoluble residue, controls the dissolution of the waste residue in the soluble residue and the insoluble residue according to different proportions of the added nitric acid, respectively measures the nickel concentration in the solution by using an atomic absorption method, and then respectively measures the nickel content in the soluble residue and the nickel content in the insoluble residue, thereby calculating the total nickel content in the total waste residue. When nitrogen trifluoride is actually produced, the loss of anode nickel is 26-28%, the content of nickel in nickel slag directly measured by dissolving nickel slag acid in the prior art is 18-19%, the loss amount of nickel is different from the actual loss amount of anode nickel, and the detection result of atomic absorption spectrum on nickel is influenced because nickel and ammonium bifluoride form a complex; the method adopts high-temperature heating of the nickel slag, the detected nickel content is 25.72-26.40%, the nickel content is close to the nickel loss amount in actual production, and the detection result of the method has guiding significance for the actual production.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the method for measuring the nickel content in the waste residue generated by nitrogen trifluoride electrolysis, the waste residue is distinguished from the insoluble residue, the nickel content is measured, and the distinguishing treatment is carried out, so that the benefit and the resource utilization of an enterprise are maximized;
(2) The method for measuring the content of nickel in waste residue generated by nitrogen trifluoride electrolysis utilizes strong acid to completely dissolve nickel in different waste residues, so that the dissolution is thorough, the material loss is small, and the result is reliable and accurate.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
The method for measuring the nickel content in the waste residue generated by nitrogen trifluoride electrolysis comprises the following steps:
(1) Weighing 2000g of waste residue generated by nitrogen trifluoride electrolysis: dissolving waste residues in 4000g of water, performing pressure filtration on 203g of solid indissolvable residues obtained by adopting a 200-mesh plate-and-frame filter press, introducing ammonia gas into filtrate until no precipitate is generated, and then performing centrifugal separation at the rotating speed of 2000r/min by adopting a centrifugal machine to obtain 596g of solid soluble residues;
(2) Determining the nickel content in the soluble slag:
a1, accurately weighing 100g of soluble slag, heating to 240 ℃, continuously calcining for 8h, stirring once every 15min in the process, and weighing the residual amount of the soluble slag to be 40g after the calcination is finished, wherein the color of the soluble slag is brick red;
b1, accurately weighing 10g of calcined soluble slag, adding 200g of distilled water, adding 154g of 65wt% nitric acid for dissolution, heating to 90 ℃ for reaction for 6h, adding water into a beaker in the process, and maintaining the liquid level at the position before heating;
c1, performing suction filtration after the reaction is finished, weighing 147mL of filtrate volume, measuring the mass concentration of nickel in the filtrate by using an atomic absorption method to be 32.95g/L, and calculating according to a formula to obtain the nickel content in the soluble slag as follows: 19.4 percent;
(3) Determining the nickel content in the refractory slag:
a2, accurately weighing 100g of refractory slag, raising the temperature of the refractory slag to 280 ℃, continuously calcining for 7h, stirring once every 15min in the process, and obtaining 86.5g of residual refractory slag after calcining, wherein the color of the refractory slag is brick red;
b2, accurately weighing 10g of calcined insoluble slag, adding 200g of distilled water, adding 62g of 65wt% nitric acid for dissolution, heating to 90 ℃ for reaction for 6h, adding water into the beaker in the process, and maintaining the liquid level at the position before heating;
c2, after the reaction is finished, carrying out suction filtration, weighing the filtrate to 190mL, measuring the mass concentration of nickel in the filtrate by using an atomic absorption method to be 27.15g/L, and calculating according to a formula to obtain the nickel content in the refractory slag as follows: 44.6 percent;
(4) The total nickel content in the waste residue from the nitrogen trifluoride electrolysis was calculated to be 25.78%.
Example 2
The method for measuring the nickel content in the waste residue generated by nitrogen trifluoride electrolysis comprises the following steps:
(1) Weighing 2000g of waste residue generated by nitrogen trifluoride electrolysis: dissolving waste residues in 5000g of water, performing pressure filtration on the obtained solid insoluble residues by using a 200-mesh plate-and-frame filter press to obtain 200g of solid insoluble residues, introducing ammonia gas into filtrate until no precipitate is generated, and then performing centrifugal separation at the rotating speed of 2500r/min by using a centrifugal machine to obtain 601g of solid soluble residues;
(2) Determining the nickel content in the soluble slag:
a1, accurately weighing 100g of soluble slag, heating to 280 ℃, continuously calcining for 5h, stirring once every 20min in the process, and weighing 36g of the residual soluble slag after the calcining is finished, wherein the color of the slag is brick red;
b1, accurately weighing 10g of calcined soluble slag, adding 200g of distilled water, adding 154g of 65wt% nitric acid for dissolution, heating to 80 ℃ for reaction for 8h, adding water into a beaker in the process, and maintaining the liquid level at the position before heating;
c1, after the reaction is finished, carrying out suction filtration, weighing 183mL of filtrate volume, measuring the mass concentration of nickel in the filtrate by using an atomic absorption method, namely 30.56g/L, and calculating the nickel content in the soluble slag according to a formula: 20.1 percent;
(3) Determining the nickel content in the refractory slag:
a2, accurately weighing 100g of refractory slag, raising the temperature of the refractory slag to 240 ℃, continuously calcining for 9h, stirring once every 20min in the process, and keeping the residual quantity of the refractory slag to be 80g after calcining to be brick red;
b2, accurately weighing 10g of calcined insoluble slag, adding 200g of distilled water, adding 62g of 65wt% nitric acid for dissolution, heating to 80 ℃ for reaction for 8 hours, adding water into the beaker in the process, and maintaining the liquid level at the position before heating;
c2, performing suction filtration after the reaction is finished, weighing the filtrate with the volume of 203mL, measuring the mass concentration of nickel in the filtrate by using an atomic absorption method to be 26.23g/L, and calculating according to a formula to obtain the nickel content in the refractory slag as follows: 42.6 percent;
(4) The total content of nickel in the waste residue produced by nitrogen trifluoride electrolysis was calculated to be 25.72%.
Example 3
The method for measuring the nickel content in the waste residue generated by nitrogen trifluoride electrolysis comprises the following steps:
(1) Weighing 2000g of waste residue generated by nitrogen trifluoride electrolysis: dissolving waste residues into 6000g of water, performing pressure filtration on 198g of solid indissolvable residues obtained by adopting a 200-mesh plate-and-frame filter press, introducing ammonia gas into filtrate until no precipitate is generated, and then performing centrifugal separation at the rotating speed of 2300r/min by adopting a centrifugal machine to obtain 603g of solid soluble residues;
(2) Determining the nickel content in the soluble slag:
a1, accurately weighing 100g of soluble slag, heating to 260 ℃, continuously calcining for 6h, stirring once every 15min in the process, and weighing 37g of the residual soluble slag after the calcination is finished, wherein the color of the slag is brick red;
b1, accurately weighing 10g of calcined soluble slag, adding 200g of distilled water, adding 154g of 65wt% nitric acid for dissolving, heating to 85 ℃, reacting for 7 hours, adding water into a beaker in the process, and maintaining the liquid level at the position before heating;
c1, performing suction filtration after the reaction is finished, weighing 167mL of filtrate volume, measuring the mass concentration of nickel in the filtrate by using an atomic absorption method to be 31.4g/L, and calculating according to a formula to obtain the nickel content in the soluble slag as follows: 19.4 percent;
(3) Determining the nickel content in the refractory slag:
a2, accurately weighing 100g of refractory slag, raising the temperature of the refractory slag to 260 ℃, continuously calcining for 8h, stirring once every 15min in the process, and obtaining 86.5g of residual refractory slag after calcining, wherein the color of the refractory slag is brick red;
b2, accurately weighing 10g of calcined insoluble slag, adding 200g of distilled water, adding 62g of 65wt% nitric acid for dissolution, heating to 90 ℃ for reaction for 6h, adding water into the beaker in the process, and maintaining the liquid level at the position before heating;
c2, performing suction filtration after the reaction is finished, weighing the filtrate with the volume of 200mL, measuring the mass concentration of nickel in the filtrate by using an atomic absorption method to be 27.6g/L, and calculating according to a formula to obtain the nickel content in the refractory slag as follows: 47.7 percent;
(4) The total content of nickel in the waste residue produced by nitrogen trifluoride electrolysis was calculated to be 26.40%.
Comparative example 1
The method for measuring the nickel content in the waste residue generated by nitrogen trifluoride electrolysis comprises the following steps:
(1) Weighing 2000g of waste residue generated by nitrogen trifluoride electrolysis: dissolving waste residues into 4000g of water, performing pressure filtration on 202g of solid indissolvable residues obtained by adopting a 200-mesh plate-and-frame filter press, introducing ammonia gas into filtrate until no precipitate is generated, and then performing centrifugal separation at the rotating speed of 2300r/min by adopting a centrifugal machine to obtain 598g of solid soluble residues;
(2) Determining the nickel content in the soluble slag:
a1, accurately weighing 10g of soluble slag, adding 200g of distilled water, adding 152g of nitric acid with the concentration of 65wt% for dissolution, heating to 90 ℃ for reaction for 6 hours, adding water into a beaker in the process, and maintaining the liquid level at the position before heating;
b1, performing suction filtration after the reaction is finished, weighing the filtrate with the volume of 142mL, measuring the mass concentration of nickel in the filtrate by using an atomic absorption method to be 11.5g/L, and calculating according to a formula to obtain the nickel content in the soluble slag as follows: 16.3 percent;
(3) Determining the nickel content in the refractory slag:
a2, accurately weighing 10g of refractory slag, adding 200g of distilled water, adding 62g of 65wt% nitric acid for dissolution, heating to 90 ℃ for reaction for 6h, adding water into a beaker in the process, and maintaining the liquid level at the position before heating;
b2, performing suction filtration after the reaction is finished, weighing the filtrate with the volume of 185mL, measuring the mass concentration of nickel in the filtrate by using an atomic absorption method to be 13.1g/L, and calculating according to a formula to obtain the nickel content in the refractory slag as follows: 24.2 percent;
(4) The total nickel content in the waste residue from the nitrogen trifluoride electrolysis was calculated to be 18.32%.
Comparative example 2
The method for measuring the nickel content in the waste residue generated by nitrogen trifluoride electrolysis comprises the following steps:
(1) Weighing 2000g of waste residue generated in nitrogen trifluoride electrolysis: dissolving waste residues in 4000g of water, performing pressure filtration on 198g of solid indissolvable residues obtained by adopting a 200-mesh plate-and-frame filter press, introducing ammonia gas into filtrate until no precipitate is generated, and then performing centrifugal separation at the rotating speed of 2300r/min by adopting a centrifugal machine to obtain 604g of solid soluble residues; (2) determining the nickel content in the soluble slag:
a1, accurately weighing 10g of soluble slag, adding 200g of distilled water, adding 159g of 65wt% nitric acid for dissolving, heating to 90 ℃, reacting for 6 hours, adding water into a beaker in the process, and maintaining the liquid level at the position before heating;
b1, performing suction filtration after the reaction is finished, weighing the volume of the filtrate to be 138mL, measuring the mass concentration of nickel in the filtrate to be 12.1g/L by using an atomic absorption method, and calculating according to a formula to obtain the nickel content in the soluble slag as follows: 16.7 percent;
(3) Determining the nickel content in the refractory slag:
a2, accurately weighing 10g of refractory slag, adding 200g of distilled water, adding 59g of nitric acid with the concentration of 65wt% for dissolution, heating to 90 ℃ for reaction for 6 hours, adding water into a beaker in the process, and maintaining the liquid level at the position before heating;
b2, performing suction filtration after the reaction is finished, weighing the filtrate with the volume of 180mL, measuring the mass concentration of nickel in the filtrate by using an atomic absorption method to be 14.4g/L, and calculating according to a formula to obtain the nickel content in the refractory slag as follows: 25.9 percent;
(4) The total content of nickel in the waste residue generated by nitrogen trifluoride electrolysis was calculated to be 18.98%.
Of course, the foregoing is only a preferred embodiment of the invention and should not be taken as limiting the scope of the embodiments of the invention. The present invention is not limited to the above examples, and equivalent changes and modifications made by those skilled in the art within the spirit of the present invention should be included in the scope of the present invention.
Claims (1)
1. A method for measuring the content of nickel in waste residue generated by nitrogen trifluoride electrolysis is characterized by comprising the following steps: firstly, distinguishing soluble slag and insoluble slag from waste residues generated in nitrogen trifluoride electrolysis, then respectively measuring the nickel content in the soluble slag and the nickel content in the insoluble slag, and finally calculating the nickel content in the waste residues generated in nitrogen trifluoride electrolysis according to the nickel content in the soluble slag and the nickel content in the insoluble slag;
the method for distinguishing soluble slag and insoluble slag of waste slag generated in nitrogen trifluoride electrolysis comprises the following steps: dissolving the waste residue in water according to the mass ratio of 1:2-1:3, and performing pressure filtration on the waste residue with 200 meshes to obtain solid which is refractory residue; introducing ammonia gas into the filtrate until no precipitate is generated, and centrifuging at 2000-2500 r/min until no water is generated, wherein the obtained solid is soluble slag;
the method for measuring the nickel content in the waste residue generated by nitrogen trifluoride electrolysis comprises the following steps of:
a1, accurately weighing and calcining soluble slag, keeping the temperature of the soluble slag at 240-280 ℃, continuously calcining for 5-8 h, and stirring once every 15-20 min in the process;
b1, accurately weighing the calcined soluble slag, adding a nitric acid solution to dissolve the soluble slag, heating to 80-90 ℃ to react for 6-8 h, adding water into a beaker in the process, and maintaining the liquid level at the position before heating;
c1, performing suction filtration after the reaction is finished, weighing the volume of the filtrate, measuring the mass concentration of nickel in the filtrate by using an atomic absorption method, and calculating to obtain the nickel content in the soluble slag;
the mass ratio of the calcined soluble slag to the nitric acid in the step b1 is 1;
the method for measuring the nickel content in the waste residue generated by nitrogen trifluoride electrolysis comprises the following steps of:
a2, accurately weighing and calcining the insoluble slag, keeping the temperature of the insoluble slag at 240-280 ℃, continuously calcining for 7-9 h, and stirring once every 15-20 min in the process;
b2, accurately weighing the calcined insoluble slag, adding a nitric acid solution to dissolve the calcined insoluble slag, heating to 80-90 ℃ to react for 6-8 h, adding water into the beaker in the process, and maintaining the liquid level at the position before heating;
c2, performing suction filtration after the reaction is finished, weighing the volume of the filtrate, measuring the mass concentration of nickel in the filtrate by using an atomic absorption method, and calculating to obtain the nickel content in the refractory slag;
the mass ratio of the refractory slag calcined in the step b2 to the nitric acid is 1:4-1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210897749.5A CN114965326B (en) | 2022-07-28 | 2022-07-28 | Method for measuring nickel content in waste residue generated by nitrogen trifluoride electrolysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210897749.5A CN114965326B (en) | 2022-07-28 | 2022-07-28 | Method for measuring nickel content in waste residue generated by nitrogen trifluoride electrolysis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114965326A CN114965326A (en) | 2022-08-30 |
| CN114965326B true CN114965326B (en) | 2022-10-21 |
Family
ID=82970298
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210897749.5A Active CN114965326B (en) | 2022-07-28 | 2022-07-28 | Method for measuring nickel content in waste residue generated by nitrogen trifluoride electrolysis |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114965326B (en) |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102213704A (en) * | 2011-03-30 | 2011-10-12 | 太原重工股份有限公司 | Method for measuring contents of silicon-calcium elements in silicon-calcium alloy |
| CN102590122A (en) * | 2012-01-17 | 2012-07-18 | 佛山市邦普循环科技有限公司 | Method for measuring cadmium content in waste nickel-cadmium battery |
| CN103575724A (en) * | 2012-08-02 | 2014-02-12 | 荆门市格林美新材料有限公司 | Method for measuring tungsten content in hard alloy |
| CN103728289A (en) * | 2013-12-16 | 2014-04-16 | 金川集团股份有限公司 | Method for rapidly measuring gold and silver in crude copper |
| CN103760051A (en) * | 2013-11-18 | 2014-04-30 | 江苏省沙钢钢铁研究院有限公司 | Method for determining content of silicon and zirconium in silicozirconium alloy |
| CN104764704A (en) * | 2015-04-22 | 2015-07-08 | 阳谷祥光铜业有限公司 | Method for determining copper phase in flash converting furnace slag |
| CN105119024A (en) * | 2015-09-18 | 2015-12-02 | 国网北京市电力公司 | Recovery method of lithium |
| CN105223307A (en) * | 2014-07-02 | 2016-01-06 | 西安航空动力股份有限公司 | A kind of detection method for element silicon volumetric method in vanadium iron |
| CN109142664A (en) * | 2018-08-27 | 2019-01-04 | 安徽寒锐新材料有限公司 | The detection method of nickel element content in a kind of high iron-containing dilval |
| CN112798575A (en) * | 2020-12-24 | 2021-05-14 | 全南晶环科技有限责任公司 | Method for measuring hafnium content in hafnium intermediate alloy |
| CN113504191A (en) * | 2021-07-02 | 2021-10-15 | 金川集团股份有限公司 | Method for measuring content of trace iron and aluminum in nickel-based solution |
| CN113533626A (en) * | 2021-06-25 | 2021-10-22 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring chloride ion content in cold-rolled chromium-containing sludge |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AUPO837197A0 (en) * | 1997-08-01 | 1997-08-28 | Centaur Mining & Exploration Limited | Selective precipitation of nickel and cobalt |
| CN110668629A (en) * | 2019-10-23 | 2020-01-10 | 洛阳黎明大成氟化工有限公司 | Treatment method of electrolytic waste residue wastewater generated by nitrogen trifluoride preparation process by electrolytic method |
| CN111875124B (en) * | 2020-06-05 | 2022-11-25 | 中船(邯郸)派瑞特种气体股份有限公司 | Treatment method of nickel-containing waste residue wastewater generated in nitrogen trifluoride preparation process |
| CN112645396B (en) * | 2020-12-11 | 2022-08-26 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for treating fluorine-containing nickel slag generated in nitrogen trifluoride preparation process |
| CN114133014B (en) * | 2021-12-13 | 2024-06-04 | 南大光电(淄博)有限公司 | Process method for recycling nickel-containing waste residues generated by electrolytic nitrogen trifluoride |
| CN114349079A (en) * | 2022-02-17 | 2022-04-15 | 中船(邯郸)派瑞特种气体股份有限公司 | Recycling treatment method for nickel slag solid waste in nitrogen trifluoride gas electrolysis production |
-
2022
- 2022-07-28 CN CN202210897749.5A patent/CN114965326B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102213704A (en) * | 2011-03-30 | 2011-10-12 | 太原重工股份有限公司 | Method for measuring contents of silicon-calcium elements in silicon-calcium alloy |
| CN102590122A (en) * | 2012-01-17 | 2012-07-18 | 佛山市邦普循环科技有限公司 | Method for measuring cadmium content in waste nickel-cadmium battery |
| CN103575724A (en) * | 2012-08-02 | 2014-02-12 | 荆门市格林美新材料有限公司 | Method for measuring tungsten content in hard alloy |
| CN103760051A (en) * | 2013-11-18 | 2014-04-30 | 江苏省沙钢钢铁研究院有限公司 | Method for determining content of silicon and zirconium in silicozirconium alloy |
| CN103728289A (en) * | 2013-12-16 | 2014-04-16 | 金川集团股份有限公司 | Method for rapidly measuring gold and silver in crude copper |
| CN105223307A (en) * | 2014-07-02 | 2016-01-06 | 西安航空动力股份有限公司 | A kind of detection method for element silicon volumetric method in vanadium iron |
| CN104764704A (en) * | 2015-04-22 | 2015-07-08 | 阳谷祥光铜业有限公司 | Method for determining copper phase in flash converting furnace slag |
| CN105119024A (en) * | 2015-09-18 | 2015-12-02 | 国网北京市电力公司 | Recovery method of lithium |
| CN109142664A (en) * | 2018-08-27 | 2019-01-04 | 安徽寒锐新材料有限公司 | The detection method of nickel element content in a kind of high iron-containing dilval |
| CN112798575A (en) * | 2020-12-24 | 2021-05-14 | 全南晶环科技有限责任公司 | Method for measuring hafnium content in hafnium intermediate alloy |
| CN113533626A (en) * | 2021-06-25 | 2021-10-22 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring chloride ion content in cold-rolled chromium-containing sludge |
| CN113504191A (en) * | 2021-07-02 | 2021-10-15 | 金川集团股份有限公司 | Method for measuring content of trace iron and aluminum in nickel-based solution |
Non-Patent Citations (3)
| Title |
|---|
| 丁二酮肟重量法测定红土镍矿低含量镍;陈诗等;《化工管理》;20170121(第03期);全文 * |
| 三氟化氮生产中废电解质镍含量的快速测定;李梅等;《化学推进剂与高分子材料》;20150528(第03期);全文 * |
| 原子吸收光谱法测定石油焦中镍和钙含量;金珊等;《石油化工》;20000720(第07期);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114965326A (en) | 2022-08-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104316643A (en) | Three-element determination method of nickel-cobalt-manganese ternary material | |
| CN109668941B (en) | Method for measuring concentrations of sulfuric acid and manganese sulfate in electrolyte aqueous solution | |
| CN114965326B (en) | Method for measuring nickel content in waste residue generated by nitrogen trifluoride electrolysis | |
| CN108503167A (en) | A method of utilizing iron and steel pickling waste liquid synthesizing new water purification agent | |
| CN112881587B (en) | Combined determination method and device for concentration of free acid and stannous in electrotinning solution | |
| Bruckenstein et al. | Chemical Stripping Analysis. Determination of Cerium (IV), Permanganate, and Iron (III) in the Micromolar Concentration Range. | |
| CN111504751A (en) | Sample pretreatment method for determining total iron content | |
| CN108375647A (en) | A kind of titanium alloy etching tank liquid chemical analysis method | |
| CN112326875A (en) | Detection method of iron-chromium redox flow battery electrolyte | |
| CN114323867A (en) | Method for analyzing and detecting uranium content in natural triuranium octoxide | |
| CN114039117A (en) | Method for selectively recovering lithium in waste lithium iron phosphate batteries | |
| Vosburgh et al. | Experiments on the Discharge Mechanism of the Manganese Dioxide Electrode | |
| Juan et al. | Simultaneous determination of trace Cu2+, Cd2+, Ni2+ and Co2+ in zinc electrolytes by oscillopolarographic second derivative waves | |
| Ravner | Analysis of Manganese Bronze | |
| CN117377868A (en) | Method for measuring content of cobaltosic oxide in lithium cobaltate | |
| Yamamura et al. | Complexometric determination of fluoride with cerium (III) | |
| CN110172592B (en) | Method for recovering beta-type cobalt oxalate from waste ternary lithium battery | |
| CN114635141B (en) | Chemical film stripping liquid for non-phosphate conversion film on steel surface, preparation method and application | |
| CN110685001A (en) | Treatment method for reducing emission of harmful substances generated by surface treatment of aluminum product | |
| CN110967239B (en) | Method for dissolving and oxidizing metallic chromium | |
| Morden | THE DETERMINATION OF THALLIUM IN THE ELECTROLYTIC WAY. | |
| CN106124495A (en) | A kind of analysis method of cadmium titanium alloy electroplating solution | |
| Maeda et al. | Prediction of dissociation constants of ammonium ion in aqueous lithium chloride solutions in terms of the Pitzer approach | |
| CN116165332A (en) | Method for testing dissolution of lattice lithium in water washing operation of ternary cathode material | |
| CN116124983A (en) | Ternary material chloride ion detection method and equipment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: No.5, No.4 Road, Gaoqing Chemical Industrial Park, Gaocheng Town, Gaoqing County, Zibo City, Shandong Province, 256300 Patentee after: Nanda Optoelectronics (Zibo) Co.,Ltd. Address before: No.5, No.4 Road, Gaoqing Chemical Industrial Park, Gaocheng Town, Gaoqing County, Zibo City, Shandong Province, 256300 Patentee before: Shandong Feiyuan Gas Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder |