CN115950845A - Method for determining tetravalent vanadium content in pickle liquor of waste denitration catalyst - Google Patents
Method for determining tetravalent vanadium content in pickle liquor of waste denitration catalyst Download PDFInfo
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Abstract
The invention relates to the technical field of waste denitration catalysts, and discloses a method for determining the content of tetravalent vanadium in an acid leaching solution of a waste denitration catalyst, which comprises the following steps: (1) Carrying out full-wavelength scanning on tetravalent vanadium standard solutions with different concentrations, and then calculating lambda 0 ‑λ 1 nm to lambda 0 +λ 1 The peak area corresponding to the nm wavelength range is used for drawing a standard curve according to the relation between the concentration of the tetravalent vanadium standard solution and the peak area, wherein lambda is 0 595 to 605 lambda 1 45 to 55; (2) And carrying out full-wavelength scanning on the acid leaching solution of the waste denitration catalyst, and determining the tetravalent vanadium content in the acid leaching solution according to the scanning result and the standard curve. The method provided by the invention can rapidly, accurately and precisely determine the content of tetravalent vanadium in the acid leaching solution of the waste denitration catalyst, thereby having good guiding function on the leaching process of the vanadium and being beneficial to the subsequent recycling of the vanadium in the acid leaching solution.
Description
Technical Field
The invention relates to the technical field of waste denitration catalysts, in particular to a method for measuring the content of tetravalent vanadium in an acid leaching solution of a waste denitration catalyst.
Background
The waste denitration catalyst contains a certain amount of vanadium, an acid leaching method is adopted for leaching the vanadium in the waste denitration catalyst, although the vanadium can be partially leached, the vanadium in the current leachate is difficult to recycle, on one hand, the reason is that the form of the vanadium in the acid leaching solution is not well understood, and the valence state and the form of the vanadium are complex and various, so that the content of the form of the vanadium, particularly the content of tetravalent vanadium in the acid leaching solution is known, and the vanadium leaching and the subsequent utilization are well guided.
However, the existing research mainly measures the total content of vanadium in the acid leaching solution, and no relevant report about the detection of the content of tetravalent vanadium in the acid leaching solution of the denitration catalyst exists. At present, the content of metal ions in a solution is mainly detected by a titration method, but the content of tetravalent vanadium in an acid leaching solution is low, the stability of the tetravalent vanadium is poor, and the valence state of the vanadium can be changed by an oxidation-reduction titration method, so that the error of detection by the titration method is large, and the method is not suitable for valence state analysis of the vanadium in the acid leaching solution in the waste denitration catalyst.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a method for determining the content of tetravalent vanadium in an acid leaching solution of a waste denitration catalyst.
In order to achieve the above object, an aspect of the present invention provides a method for determining a content of tetravalent vanadium in an acid leach solution of a waste denitration catalyst, the method comprising the steps of:
(1) The tetravalent vanadium standard solution with different concentrations is scanned at full wavelength and then measuredCalculating lambda 0 -λ 1 nm to lambda 0 +λ 1 The peak area corresponding to the nm wavelength range is used for drawing a standard curve according to the relation between the concentration of the tetravalent vanadium standard solution and the peak area, wherein lambda is 0 595 to 605 lambda 1 45 to 55;
(2) And carrying out full-wavelength scanning on the acid leaching solution of the waste denitration catalyst, and determining the content of tetravalent vanadium in the acid leaching solution according to the scanning result and the standard curve.
Preferably, in the step (1), the preparation process of the standard solution of tetravalent vanadium comprises: mixing an acid solution with the pH of 2-6 with vanadyl sulfate.
Preferably, step (1) comprises:
s11, carrying out full-wavelength scanning H1 on tetravalent vanadium standard solutions with different concentrations;
s12, performing full-wavelength scanning H2 on the acid solution;
s13, taking H2 as a reference, subtracting H1 from H2 to obtain a spectrogram H3, and calculating lambda in H3 0 -λ 1 nm to lambda 0 +λ 1 And fitting the peak area of the obtained peak in the nm wavelength band to obtain a standard peak area S0, and then drawing a standard curve according to the relation between the concentration of the tetravalent vanadium standard solution and the standard peak area S0.
Preferably, step (2) comprises:
s21, carrying out acid leaching on the waste denitration catalyst by using a soaking solution, and carrying out full-wavelength scanning on the obtained acid leaching solution to obtain a spectrogram P1;
s22, carrying out full-wavelength scanning on the soak solution to obtain a spectrogram P2;
s23, taking P2 as a reference, carrying out difference on the spectrograms P1 and P2 to obtain a spectrogram P3, and calculating lambda in the spectrogram P3 0 -λ 1 nm to lambda 0 +λ 1 And fitting the peak area of the obtained peak in the nm wavelength range to obtain a peak area P0, and then determining the tetravalent vanadium content in the pickle liquor according to the peak area P0 and a standard curve.
Preferably, in step (1), the acid solution is a dilute sulfuric acid solution.
Preferably, the addition amount of the vanadyl sulfate is 0.5 to 20 times of the total mass of vanadium elements in the pickle liquor.
Preferably, in the step (2), the vanadium content in the waste denitration catalyst is not less than 0.2wt%.
Preferably, in the step (2), the total content of vanadium in the pickle liquor is not less than 0.01mg/L.
Preferably, in the step (2), the soaking solution used for acid leaching is one or more selected from oxalic acid, nitric acid, hydrochloric acid and citric acid.
Preferably, the scanning wavelength range is 400 to 1000nm.
The method provided by the invention can be used for rapidly, accurately and precisely measuring the content of tetravalent vanadium in the acid leaching solution of the waste denitration catalyst, and has a good guiding function on the leaching and subsequent utilization of the vanadium.
Drawings
FIG. 1 is the full wavelength scan of the pickle liquors of examples 2, 3 and 5, where A is example 2, B is example 5 and C is example 3.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for determining the content of tetravalent vanadium in an acid leaching solution of a waste denitration catalyst, which comprises the following steps:
(1) Carrying out full-wavelength scanning on tetravalent vanadium standard solutions with different concentrations, and then calculating lambda 0 -λ 1 nm to lambda 0 +λ 1 Peak area corresponding to nm wavelength band according toDrawing a standard curve according to the relation of the concentration of the vanadium valence standard solution and the peak area, wherein lambda is 0 595 to 605 lambda 1 45 to 55;
(2) And carrying out full-wavelength scanning on the acid leaching solution of the waste denitration catalyst, and determining the tetravalent vanadium content in the acid leaching solution according to the scanning result and the standard curve.
In one embodiment, the concentration of the tetravalent vanadium standard solution is: 1mg/L, 4mg/L, 10mg/L, 15mg/L and 20mg/L.
The research shows that the alpha is 0 nm (i.e., around 600 nm) is the characteristic absorption peak of tetravalent vanadium, and therefore, by using λ 0 nm as the central peak, λ 1 And nm is the radius, the peak area is calculated by fitting, and then the relationship is established between the peak area and the concentration of tetravalent vanadium, so that the interference of vanadium ions of other valence states in the pickle liquor on the detection result can be effectively eliminated, and the accuracy of the detection result is high.
In a most preferred embodiment, λ 0 Is 600nm, lambda 1 Is 50nm, namely, in the step (1), the peak area corresponding to the wavelength range of 550 to 650nm is calculated.
The reaction mechanism of the vanadium leaching stage can be better inferred by detecting the content of tetravalent vanadium, so that a better leaching recovery technical scheme is better assisted to be formulated, and vanadium in the catalyst is separated; meanwhile, the valence state of the vanadium is clear, so that the subsequent immobilization or product utilization can be facilitated.
In a preferred embodiment, in step (1), the preparation process of the standard solution of tetravalent vanadium comprises: mixing an acid solution with the pH of 2-6 with vanadyl sulfate to dissolve the vanadyl sulfate in the acid solution.
In order to make the detection result more accurate, in a preferred embodiment, the peak areas in step (1) and step (2) are subtracted from the peak area corresponding to the blank control.
In specific implementation, the step (1) comprises the following steps:
s11, carrying out full-wavelength scanning H1 on tetravalent vanadium standard solutions with different concentrations;
step S12, performing full-wavelength scanning H2 on the acid solution;
step S13, taking H2 as a reference, subtracting H1 from H2 to obtain a spectrogram H3, and calculating lambda in H3 0 -λ 1 nm to lambda 0 +λ 1 And fitting the peak area of the obtained peak in the nm wavelength range to obtain a standard peak area S0, and then drawing a standard curve according to the relation between the concentration of the tetravalent vanadium standard solution and the standard peak area S0.
In specific implementation, the step (2) comprises the following steps:
step S21, carrying out acid leaching on the waste denitration catalyst by using a soaking solution, and carrying out full-wavelength scanning on the obtained acid leaching solution to obtain a spectrogram P1;
s22, carrying out full-wavelength scanning on the soak solution to obtain a spectrogram P2;
step S23, taking P2 as a reference, subtracting the spectrograms P1 and P2 to obtain a spectrogram P3, and calculating lambda in the spectrogram P3 0 -λ 1 nm to lambda 0 +λ 1 And fitting the peak area of the obtained peak in the nm wavelength range to obtain a peak area P0, and then determining the tetravalent vanadium content in the pickle liquor according to the peak area P0 and a standard curve. That is, in the present invention, S0= S1-S2, and P0= P1-P2.
In a preferred embodiment, the acid solution is a dilute sulfuric acid solution. In specific implementation, the preparation method of the acid solution is as follows: and (3) dropwise adding dilute sulfuric acid into deionized water to adjust the pH to 1 to 2. More preferably, the concentration of the dilute sulfuric acid is 0.01 to 2mol/L, and more preferably 0.01 to 0.04mol/L.
In a preferred embodiment, the addition amount of the vanadyl sulfate is 0.5 to 20 times of the total mass of vanadium elements in the pickle liquor,
in a preferred embodiment, in step (2), the vanadium content in the waste denitration catalyst is not less than 0.2wt%, and specifically, for example, may be 0.2wt%, 0.3wt%, 0.46wt%, 0.5wt%, or 0.6wt%.
In a preferred embodiment, in step (2), the total vanadium content in the pickle liquor is not less than 0.01mg/L, and specifically, for example, may be 0.01mg/L, 0.11mg/L, 2.45mg/L, 3mg/L, 4mg/L, 4.88mg/L or 7mg/L.
In a preferred embodiment, in the step (2), the soaking solution used in the acid leaching is one or more selected from oxalic acid, nitric acid, hydrochloric acid and citric acid.
In a preferred embodiment, the scanning wavelength range is from 400 to 1000nm.
The present invention will be described in detail below by way of examples, but the scope of the present invention is not limited thereto.
In the following examples, the instrument used for full wavelength scanning was 752NPlus uv spectrophotometer, the wavelength range was 400-1000nm, and the vanadium content in the waste denitration catalyst was 0.46wt%.
Example 1
This example illustrates the determination of the standard curve according to the invention.
(1) Dropwise adding dilute sulfuric acid into deionized water to adjust the pH value to 4 to obtain a dilute sulfuric acid solution, dissolving vanadyl sulfate monohydrate with different masses into the dilute sulfuric acid solution, diluting to 1000mL to obtain tetravalent vanadium standard solutions with the concentrations of 1mg/L, 4mg/L, 10mg/L, 15mg/L and 20mg/L, and respectively scanning the tetravalent vanadium standard solutions at full wavelength to obtain a spectrogram H1;
(2) The leaching comparison system is a dilute sulfuric acid solution without vanadyl sulfate, the dilute sulfuric acid solution is diluted to 1000mL, and the dilute sulfuric acid solution is scanned at full wavelength to obtain a spectrogram H2;
(3) Subtracting the spectrograms H1 and H2 to obtain a spectrogram H3, and calculating the spectrogram in the H3 to be 550-650nm (namely lambda) 0 Is 600, λ 1 50) peak area of the peak obtained by fitting the wavelength band to obtain peak area S0; then taking the concentration of the tetravalent vanadium standard solution as an abscissa and the standard peak area as an ordinate to obtain a standard curve S =4.7732C +0.1653 2 =0.9945。
Example 2
This example is provided to illustrate the method for determining the content of tetravalent vanadium in the pickle liquor of the waste denitration catalyst according to the present invention.
(1) Soaking 2g of waste denitration catalyst in 20mL of oxalic acid with the concentration of 2mol/L for 4h at 80 ℃, washing (washing the catalyst and soaking the inner wall of a container used for soaking) after the reaction is finished, filtering and metering the volume to 1000mL to obtain pickle liquor, and scanning the pickle liquor at full wavelength to obtain a spectrogram P1;
(2) Diluting 20mL of oxalic acid with the concentration of 2mol/L to 1000mL by using deionized water, and then carrying out full-wavelength scanning to obtain a spectrum P2;
(3) Obtaining P3 by subtracting the spectrograms P1 and P2, and calculating 550 to 650nm (namely lambda) in the P3 0 Is 600, λ 1 50) peak area of the peak obtained by wavelength band fitting (shown as A in FIG. 1), and obtaining peak area P0; then, according to the peak area P0 and the standard curve in the example 1, the content of tetravalent vanadium in the pickle liquor is calculated.
Example 3
This example is provided to illustrate the method for determining the content of tetravalent vanadium in the pickle liquor of the waste denitration catalyst according to the present invention.
(1) Soaking 2g of waste denitration catalyst in 20mL of nitric acid with the concentration of 6mol/L for 5h at 80 ℃, washing and filtering after the reaction is finished, then fixing the volume to 1000mL to obtain pickle liquor, and scanning the pickle liquor at full wavelength to obtain a spectrogram P1;
(2) Diluting 20mL of nitric acid with the concentration of 6mol/L to 1000mL by using deionized water, and then carrying out full-wavelength scanning to obtain a spectrogram P2;
(3) The peak area P1 and the peak area P2 are differed to obtain a spectrogram P3, and in the spectrogram P3, the calculation is carried out at 550 to 650nm (namely, lambda) 0 Is 600, λ 1 50) the peak area of the obtained peak (shown as C in figure 1) is fitted to the wavelength band to obtain the peak area P0, and then the tetravalent vanadium content in the pickle liquor is calculated according to the peak area P0 and the standard curve in example 1.
Example 4
This example is provided to illustrate the method for determining the content of tetravalent vanadium in the pickle liquor of the waste denitration catalyst according to the present invention.
(1) Soaking 2g of waste denitration catalyst in 20mL of hydrochloric acid with the concentration of 4mol/L for 2h at 80 ℃, washing and filtering after the reaction is finished, then fixing the volume to 1000mL to obtain pickle liquor, and scanning the pickle liquor at full wavelength to obtain a spectrogram P1;
(2) Diluting 20mL of hydrochloric acid with the concentration of 4mol/L to 1000mL, and then carrying out full-wavelength scanning to obtain a spectrogram P2;
(3) The difference is made between the spectrograms P1 and P2 to obtain a spectrogram P3, and in the spectrogram P3, the calculation is carried out for 550 to 650nm (namely, lambda) 0 Is 600, λ 1 50) the peak area of the obtained peak is fitted in the wavelength range to obtain the peak area P0, and then the tetravalent vanadium content in the pickle liquor is calculated according to the peak area P0 and the standard curve in the embodiment 1.
Example 5
This example is intended to illustrate the method of determining the tetravalent vanadium content in the pickle liquor of a spent denitration catalyst according to the present invention.
(1) Soaking 2g of waste denitration catalyst in 20mL of citric acid with the concentration of 4mol/L for 2h at 80 ℃, washing and filtering after the reaction is finished, then metering the volume to 1000mL to obtain pickle liquor, and scanning the pickle liquor at full wavelength to obtain a spectrogram P1;
(2) Diluting 20mL of citric acid with concentration of 4mol/L to 1000mL by using deionized water, and then carrying out full-wavelength scanning to obtain a spectrogram P2;
(3) The spectrograms P1 and P2 are differenced to obtain a spectrogram P3, and in the spectrogram P3, the calculation is carried out at 550 to 650nm (namely, lambda is 0 Is 600, λ 1 50) the peak area of the obtained peak (shown as B in figure 1) is fitted to the wavelength band to obtain the peak area P0, and then the tetravalent vanadium content in the pickle liquor is calculated according to the peak area P0 and the standard curve in example 1.
Comparative example 1
(1) Gradually dropwise adding dilute sulfuric acid into deionized water to adjust the pH value to 4 to obtain a dilute sulfuric acid solution, dissolving vanadyl sulfate monohydrate with different masses into the dilute sulfuric acid solution, diluting to 1000mL to obtain tetravalent vanadium standard solutions with the concentrations of 1mg/L, 4mg/L, 10mg/L, 15mg/L and 20mg/L, and detecting the absorbance S1 of the tetravalent vanadium standard solution at 600 nm;
(2) The leaching contrast system is a dilute sulfuric acid solution without vanadyl sulfate, the dilute sulfuric acid solution is diluted to 1000mL, and the absorbance S2 of the dilute sulfuric acid solution at 600nm is detected;
(3) The absorbances S1 and S2 are subtracted to obtain a standard absorbance S0 (namely S0= S1-S2), the concentration of the tetravalent vanadium standard solution is used as an abscissa, the standard absorbance S0 is used as an ordinate, and a standard curve S =0.6844b +0.0012 is obtained 2 =0.7823。
From R 2 As can be seen, the linear relationship between the absorbance and the concentration of tetravalent vanadium is poor, which indicates that the concentration of tetravalent vanadium is measured by directly using the relationship between the absorbance and the concentration of tetravalent vanadium, and the error is large.
Comparative example 2
Carried out as described in example 1, except that 0 Is 650nm,. Lambda. 1 At 50nm, the standard curve was calculated as: s =10.3329C 0.3452 2 =0.5622。
From R 2 As can be seen, when the peak areas corresponding to the wavelength bands of 600 to 700nm are tested, the linear relationship between the peak areas and the tetravalent vanadium concentration is poor.
Comparative example 3
Carried out as described in example 1, except that 0 700nm,. Lambda. 1 At 50nm, the standard curve was calculated as: s =12.4235C 0.2232 2 =0.3829。
From R 2 The value can be seen when 0 When the test shows that the peak area corresponds to the wavelength range of 650 to 750nm, the linear relation between the peak area and the tetravalent vanadium concentration is poor.
Test example 1
1. The test results of the above examples 2 to 5 (3 parallel tests) are shown in table 1, and the relative standard deviation was calculated from the test results.
TABLE 1
As can be seen from Table 1, the standard curve drawn by the detection method provided by the invention has good fitting degree, good applicability to the determination of tetravalent vanadium in leachate of different acid leaching systems, and good stability, and the relative standard deviation is below 5%, which indicates that the repeated determination results are consistent.
2. The total vanadium content of the pickle liquor was tested using an inductively coupled plasma emission spectroscopy instrument and the results are shown in table 2 below.
TABLE 2
As can be seen from the results shown in tables 1 and 2, the leaching of tetravalent vanadium can be facilitated by the acid leaching system using oxalic acid, while the leaching of all vanadium can be facilitated by the acid leaching system using hydrochloric acid. By measuring tetravalent vanadium in the acid leaching solution, data reference is provided for subsequent utilization of the acid leaching solution, and a corresponding acid leaching system, acid leaching conditions and the like can be selected better according to the requirements of the subsequent utilization of the acid leaching solution.
Test example 2
The accuracy of the method provided by the present invention is demonstrated below by taking the hydrochloric acid system (i.e., example 4) as an example.
The 1L acid leaching solution of example 4 was selected, different amounts of tetravalent vanadium ion standard solution (prepared with 4mol/L hydrochloric acid) for IL were added, the tetravalent vanadium ion concentration was measured according to the detection method of example 4, each sample was measured 3 times, and the normalized recovery rate was calculated by taking the average value: the results of (measurement value of the spiked sample-measurement value of the sample) ÷ spiked amount × 100% are shown in table 3.
TABLE 3
As can be seen from Table 3, the normalized recovery rate of the method provided by the invention is between 91% and 105%, which shows that the method provided by the invention is feasible and has high accuracy.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for determining the content of tetravalent vanadium in acid leaching solution of a waste denitration catalyst is characterized by comprising the following steps:
(1) Carrying out full-wavelength scanning on tetravalent vanadium standard solutions with different concentrations, and then calculating lambda 0 -λ 1 nm to lambda 0 +λ 1 The peak area corresponding to the nm wavelength range is used for drawing a standard curve according to the relation between the concentration of the tetravalent vanadium standard solution and the peak area, wherein lambda is 0 595 to 605 lambda 1 45 to 55;
(2) And carrying out full-wavelength scanning on the acid leaching solution of the waste denitration catalyst, and determining the content of tetravalent vanadium in the acid leaching solution according to the scanning result and the standard curve.
2. The method according to claim 1, wherein in the step (1), the preparation process of the standard solution of tetravalent vanadium comprises: mixing an acid solution with the pH of 2-6 with vanadyl sulfate.
3. The method of claim 2, wherein step (1) comprises:
s11, carrying out full-wavelength scanning H1 on tetravalent vanadium standard solutions with different concentrations;
s12, performing full-wavelength scanning H2 on the acid solution;
s13, taking H2 as a reference, subtracting H1 from H2 to obtain a spectrogram H3, and calculating lambda in H3 0 -λ 1 nm to lambda 0 +λ 1 And fitting the peak area of the obtained peak in the nm wavelength range to obtain a standard peak area S0, and then drawing a standard curve according to the relation between the concentration of the tetravalent vanadium standard solution and the standard peak area S0.
4. The method of claim 3, wherein step (2) comprises:
s21, carrying out acid leaching on the waste denitration catalyst by using a soaking solution, and carrying out full-wavelength scanning on the obtained acid leaching solution to obtain a spectrogram P1;
s22, carrying out full-wavelength scanning on the soak solution to obtain a spectrogram P2;
s23, taking P2 as a reference, carrying out difference on the spectrograms P1 and P2 to obtain a spectrogram P3, and calculating lambda in the spectrogram P3 0 -λ 1 nm to lambda 0 +λ 1 And fitting the peak area of the obtained peak in the nm wavelength range to obtain a peak area P0, and then determining the tetravalent vanadium content in the pickle liquor according to the peak area P0 and a standard curve.
5. The method according to claim 2, wherein in step (1), the acid solution is a dilute sulfuric acid solution.
6. The method according to claim 2, wherein the addition amount of the vanadyl sulfate is 0.5 to 20 times of the total mass of vanadium elements in the pickle liquor.
7. The method according to claim 1, wherein in the step (2), the vanadium content in the waste denitration catalyst is not less than 0.2wt%.
8. The method of claim 1, wherein in step (2), the total vanadium content in the pickle liquor is not less than 0.01mg/L.
9. The method according to claim 1, wherein in the step (2), the soaking solution used for the acid leaching is one or more selected from oxalic acid, nitric acid, hydrochloric acid and citric acid.
10. The method of claim 1, wherein the scanning wavelength range is 400 to 1000nm.
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| CN109596556A (en) * | 2018-12-13 | 2019-04-09 | 山西大学 | The method of Pb In Exhausted Water ion concentration is quickly and easily measured using Quercetin |
| CN110161137A (en) * | 2019-05-21 | 2019-08-23 | 华中科技大学 | A method of measurement sodium-iron-chlorophyllin |
| WO2022134255A1 (en) * | 2020-12-23 | 2022-06-30 | 广东省科学院生态环境与土壤研究所 | Method for measuring contents of trivalent stibium and pentavalent stibium by means of liquid chromatography combined with atomic fluorescence spectrometry |
| CN112730292A (en) * | 2020-12-28 | 2021-04-30 | 大连博融新材料有限公司 | Method for determining iron content in ferrovanadium solution by EDTA complexation-hydrogen peroxide chromogenic matrix matching photometry |
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