CN115950845B - Method for determining tetravalent vanadium content in pickle liquor of waste denitration catalyst - Google Patents
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Abstract
The invention relates to disposal ofThe technical field of denitration catalysts, discloses a method for determining tetravalent vanadium content in pickle liquor of a waste denitration catalyst, which comprises the following steps: (1) Scanning all wave length of tetravalent vanadium standard solution with different concentrations, and calculating lambda 0 ‑λ 1 nm to lambda 0 +λ 1 Drawing a standard curve according to the relation between the concentration of tetravalent vanadium standard solution and the peak area, wherein lambda is the peak area corresponding to the nm wavelength band 0 595-605 lambda 1 45-55; (2) And (3) carrying out full-wavelength scanning on the pickle liquor of the waste denitration catalyst, and determining the tetravalent vanadium content in the pickle liquor according to a scanning result and the standard curve. The method provided by the invention can be used for rapidly, accurately and highly accurately measuring the content of tetravalent vanadium in the pickling solution of the waste denitration catalyst, thereby having a good guiding effect on the leaching process of vanadium and being beneficial to the subsequent recycling of vanadium in the pickling solution.
Description
Technical Field
The invention relates to the technical field of waste denitration catalysts, in particular to a method for measuring tetravalent vanadium content in pickle liquor of a waste denitration catalyst.
Background
The waste denitration catalyst contains a certain amount of vanadium, the leaching of vanadium in the waste denitration catalyst is carried out by adopting an acid leaching method, although vanadium can be partially leached, vanadium in the leaching solution is difficult to recycle subsequently at present, on one hand, the reason is that the morphology of vanadium in the acid leaching solution is not enough, and the valence state and the form of vanadium are complex and various, so that the content of vanadium in the acid leaching solution, particularly tetravalent vanadium, is known, and the leaching and subsequent utilization of vanadium are better guided.
However, the prior research mainly detects the total content of vanadium in the pickle liquor, but no related report on detecting the tetravalent vanadium content in the denitration catalyst pickle liquor exists. At present, a titration method is mainly used for detecting the content of metal ions in a solution, but the content of tetravalent vanadium in a pickling solution is low, the stability of tetravalent vanadium is poor, and the redox titration method can cause the change of vanadium valence, so that the error of detection by the titration method can be large, and the titration method is not suitable for the valence analysis of vanadium in the pickling solution in a waste denitration catalyst.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a method for determining the tetravalent vanadium content in the pickle liquor of a waste denitration catalyst.
In order to achieve the above object, the present invention provides a method for determining the tetravalent vanadium content in an pickle liquor of a waste denitration catalyst, the method comprising the steps of:
(1) Scanning all wave length of tetravalent vanadium standard solution with different concentrations, and calculating lambda 0 -λ 1 nm to lambda 0 +λ 1 Drawing a standard curve according to the relation between the concentration of tetravalent vanadium standard solution and the peak area, wherein lambda is the peak area corresponding to the nm wavelength band 0 595-605 lambda 1 45-55;
(2) And (3) carrying out full-wavelength scanning on the pickle liquor of the waste denitration catalyst, and determining the tetravalent vanadium content in the pickle liquor according to a scanning result and the standard curve.
Preferably, in the step (1), the preparation process of the tetravalent vanadium standard solution comprises the following steps: and mixing the acid solution with the pH value of 2-6 with vanadyl sulfate.
Preferably, step (1) comprises:
s11, performing full-wavelength scanning on tetravalent vanadium standard solutions with different concentrations to obtain H1;
s12, carrying out full-wavelength scanning H2 on the acid solution;
s13, taking H2 as a reference, differencing H1 and H2 to obtain a spectrogram H3, and calculating lambda in the 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 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-wave scanning on the obtained pickling solution to obtain a spectrogram P1;
s22, carrying out full-wavelength scanning on the soaking solution to obtain a spectrogram P2;
s23, taking P2 as a reference, and differencing the spectrograms P1 and P2 to obtain a spectrogram P3, wherein lambda is calculated 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 band to obtain a peak area P0, and determining the tetravalent vanadium content in the pickling solution 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 adding amount of vanadyl sulfate is 0.5-20 times of the total mass of vanadium element 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 vanadium content in the pickle liquor is not less than 0.01mg/L.
Preferably, 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.
Preferably, the scanning wavelength range is 400-1000 nm.
The method provided by the invention can be used for rapidly, accurately and highly accurately measuring the content of tetravalent vanadium in the pickle liquor of the waste denitration catalyst, and has good guiding effect on leaching and subsequent utilization of vanadium.
Drawings
FIG. 1 is the full wavelength scan of the pickling solutions in examples 2, 3 and 5, wherein A is example 2, B is example 5, and C is example 3.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The invention provides a method for determining tetravalent vanadium content in pickle liquor of a waste denitration catalyst, which comprises the following steps:
(1) Scanning all wave length of tetravalent vanadium standard solution with different concentrations, and calculating lambda 0 -λ 1 nm to lambda 0 +λ 1 Drawing a standard curve according to the relation between the concentration of tetravalent vanadium standard solution and the peak area, wherein lambda is the peak area corresponding to the nm wavelength band 0 595-605 lambda 1 45-55;
(2) And (3) carrying out full-wavelength scanning on the pickle liquor of the waste denitration catalyst, and determining the tetravalent vanadium content in the pickle liquor according to a 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.
Through research, lambda 0 nm (i.e., around 600 nm) is a characteristic absorption peak of tetravalent vanadium, and therefore, by lambda 0 nm as central peak, lambda 1 nm is the radius to fit and calculate the peak area, and then the peak area is related to the tetravalent vanadium concentration, so that the interference of vanadium ions in other valence states in the pickle liquor on the detection result can be effectively eliminated, and the method is characterized in thatThe accuracy of the detection result is high.
In a most preferred embodiment λ 0 600nm, lambda 1 The peak area corresponding to the wavelength band of 550-650 nm is calculated as 50nm, namely in the step (1).
The reaction mechanism of the vanadium leaching stage can be better deduced by detecting the content of tetravalent vanadium, so that better leaching recovery technical schemes can be better assisted to be formulated, and vanadium in the catalyst is separated; meanwhile, the valence state of vanadium can be clearly beneficial to preparing the subsequent immobilization or product utilization.
In a preferred embodiment, in step (1), the preparation process of the tetravalent vanadium standard solution comprises: and mixing the acid solution with the pH value 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 by the peak area corresponding to the blank.
In specific implementation, the step (1) includes:
s11, performing full-wavelength scanning H1 on tetravalent vanadium standard solutions with different concentrations;
step S12, carrying out full-wavelength scanning H2 on the acid solution;
step S13, taking H2 as a reference, differencing H1 and 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 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) includes:
step S21, pickling the waste denitration catalyst by using a soaking solution, and full-wave scanning the obtained pickling solution to obtain a spectrogram P1;
step S22, carrying out full-wavelength scanning on the soaking solution to obtain a spectrogram P2;
step S23, taking P2 as a reference, taking difference between the spectrograms P1 and P2 to obtain a spectrogram P3, in P3,calculating lambda 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 peak area P0, and determining the tetravalent vanadium content in the pickling solution according to the peak area P0 and a standard curve. That is, in the present invention, s0=s1-S2, 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 comprises the following steps: and adding dilute sulfuric acid into deionized water dropwise to adjust the pH to 1-2. Further preferably, the concentration of the dilute sulfuric acid is 0.01-2 mol/L, more preferably 0.01-0.04 mol/L.
In a preferred embodiment, the adding amount of vanadyl sulfate is 0.5-20 times of the total mass of vanadium element in the pickle liquor,
in a preferred embodiment, in the step (2), the vanadium content of the waste denitration catalyst is not less than 0.2wt%, 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 pickling solution 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 for 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 400-1000 nm.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
In the following example, the total wavelength scanning used was 752NPlus ultraviolet spectrophotometer with wavelength range of 400-1000nm, and the vanadium element content in the waste denitration catalyst was 0.46wt%.
Example 1
This example is intended to illustrate the determination of a standard curve according to the invention.
(1) Adding dilute sulfuric acid dropwise into deionized water to adjust the pH to 4 to obtain a dilute sulfuric acid solution, dissolving vanadyl sulfate monohydrate with different mass into the dilute sulfuric acid solution, diluting to 1000mL to obtain tetravalent vanadium standard solutions with the concentration of 1mg/L, 4mg/L, 10mg/L, 15mg/L and 20mg/L, and respectively performing full-wavelength scanning on the tetravalent vanadium standard solutions to obtain a spectrogram H1;
(2) The leaching contrast system is a dilute sulfuric acid solution without adding vanadyl sulfate, and is diluted to 1000mL, and full-wave scanning is carried out on the dilute sulfuric acid solution to obtain a spectrogram H2;
(3) The spectra H1 and H2 are differenced to obtain a spectrum H3, and in the spectrum H3, 550-650 nm (i.e., lambda 0 600 lambda 1 50) fitting the peak area of the obtained peak in the wavelength band to obtain a peak area S0; then, the concentration of the tetravalent vanadium standard solution is taken as an abscissa, the standard peak area is taken as an ordinate, and a standard curve S=4.7732C+0.1653 and R are obtained 2 =0.9945。
Example 2
This example is used to illustrate the method of the invention for determining the tetravalent vanadium content in the pickle liquor of the spent denitration catalyst.
(1) Soaking 2g of waste denitration catalyst with 20mL of oxalic acid with the concentration of 2mol/L for 4 hours at the soaking temperature of 80 ℃, washing (washing the catalyst and the inner wall of a container used for soaking) after the reaction is finished, filtering to reach 1000mL of constant volume to obtain pickling liquid, and performing full-wavelength scanning on the pickling liquid 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 performing full-wavelength scanning to obtain a spectrum P2;
(3) The spectra P1 and P2 are differenced to obtain P3, and in P3, 550-650 nm (i.e. lambda 0 600 lambda 1 50) peak areas of the obtained peaks (shown as a in fig. 1) are fitted to each other to obtain peak areas P0; the tetravalent vanadium content in the pickle liquor was then calculated from the peak area P0 and the standard curve in example 1.
Example 3
This example is used to illustrate the method of the invention for determining the tetravalent vanadium content in the pickle liquor of the spent denitration catalyst.
(1) Soaking 2g of waste denitration catalyst with 20mL of nitric acid with the concentration of 6mol/L for 5h at the soaking temperature of 80 ℃, washing and filtering after the reaction is finished, and then fixing the volume to 1000mL to obtain pickling solution, and performing full-wavelength scanning on the pickling solution 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 performing full-wavelength scanning to obtain a spectrogram P2;
(3) The peak area P1 and the peak area P2 are subjected to difference to obtain a spectrum P3, and in the spectrum P3, 550-650 nm (namely lambda is calculated 0 600 lambda 1 50) peak area of the obtained peak (shown as C in fig. 1) was fitted to the wavelength band to obtain peak area P0, and then the tetravalent vanadium content in the pickle liquor was calculated from peak area P0 and the standard curve in example 1.
Example 4
This example is used to illustrate the method of the invention for determining the tetravalent vanadium content in the pickle liquor of the spent denitration catalyst.
(1) Soaking 2g of waste denitration catalyst in 20mL of hydrochloric acid with the concentration of 4mol/L for 2h at the soaking temperature of 80 ℃, washing and filtering after the reaction is finished, and then fixing the volume to 1000mL to obtain pickling solution, and performing full-wavelength scanning on the pickling solution to obtain a spectrogram P1;
(2) Diluting 20mL of hydrochloric acid with the concentration of 4mol/L to 1000mL, and then performing full-wavelength scanning to obtain a spectrogram P2;
(3) The spectra P1 and P2 are differenced to obtain a spectrum P3, and in P3, 550-650 nm (i.e., lambda 0 600 lambda 1 50) peak area of the obtained peak was fitted to a wavelength band to obtain peak area P0, and then tetravalent vanadium content in the pickle liquor was calculated from peak area P0 and the standard curve in example 1.
Example 5
This example is used to illustrate the method of the invention for determining the tetravalent vanadium content in the pickle liquor of the spent denitration catalyst.
(1) Soaking 2g of waste denitration catalyst with 20mL of citric acid with concentration of 4mol/L for 2h at 80 ℃, washing and filtering after the reaction is finished, and then fixing the volume to 1000mL to obtain pickling solution, and performing full-wavelength scanning on the pickling solution to obtain a spectrogram P1;
(2) Diluting 20mL of citric acid with the concentration of 4mol/L to 1000mL by deionized water, and then performing full-wavelength scanning to obtain a spectrogram P2;
(3) The spectra P1 and P2 are differenced to obtain a spectrum P3, and in P3, 550-650 nm (i.e., lambda 0 600 lambda 1 50) peak area of the obtained peak (shown as B in fig. 1) was fitted to the wavelength band to obtain peak area P0, and then the tetravalent vanadium content in the pickle liquor was calculated from peak area P0 and the standard curve in example 1.
Comparative example 1
(1) Adding dilute sulfuric acid dropwise into deionized water to adjust the pH 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 comparison system is a dilute sulfuric acid solution without adding vanadyl sulfate, and is diluted to 1000mL, and the absorbance S2 of the dilute sulfuric acid solution at 600nm is detected;
(3) The absorbance S1 and the absorbance S2 are subjected to difference to obtain a standard absorbance S0 (namely S0=S1-S2), the concentration of the tetravalent vanadium standard solution is taken as an abscissa, the standard absorbance S0 is taken as an ordinate, and a standard curve S=0.6844b+0.0012 and R are obtained 2 =0.7823。
From R 2 The value can be seen that the linear relation between the absorbance and the concentration of tetravalent vanadium is poor, which indicates that the relation between the absorbance and the concentration of tetravalent vanadium is directly used for measuring the concentration of tetravalent vanadium, and the error is larger.
Comparative example 2
The procedure is carried out as described in example 1, except that λ 0 650nm, lambda 1 50nm, calculated as standard curve: s=10.3329c+0.3452, r 2 =0.5622。
From R 2 The value shows that when the peak area corresponding to the wavelength band of 600-700 nm is tested, the linear relation between the peak area and the tetravalent vanadium concentration is poor.
Comparative example 3
The procedure is carried out as described in example 1, except that λ 0 700nm, lambda 1 50nm, calculated as standard curve: s=12.4235c+0.2232, r 2 =0.3829。
From R 2 The value can be seen when lambda 0 The test shows that when the peak area corresponding to the wavelength band of 650-750 nm is measured, the linear relation between the peak area and the tetravalent vanadium concentration is poor.
Test example 1
1. The test results (3 times in parallel) of the above examples 2 to 5 are shown in table 1, and the relative standard deviation is 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 determination of tetravalent vanadium in leaching solutions of different acid leaching systems, and good stability, and the relative standard deviation is below 5%, which indicates that repeated determination results are consistent.
2. The total vanadium content of the pickle liquor was measured using an inductively coupled plasma emission spectrometry instrument and the results are shown in table 2 below.
TABLE 2
It can be seen from the results of tables 1 and 2 that the leaching of tetravalent vanadium can be facilitated by using an acid leaching system of oxalic acid, while the leaching of all vanadium can be facilitated by using an acid leaching system of hydrochloric acid. By measuring tetravalent vanadium in the pickle liquor, data reference is provided for subsequent utilization of the pickle liquor, and corresponding acid leaching systems, acid leaching conditions and the like can be better selected according to the requirement of subsequent utilization of the pickle liquor.
Test example 2
The accuracy of the method provided by the present invention is verified by taking a hydrochloric acid system (i.e., example 4) as an example.
1L of pickle liquor of example 4 is selected, different amounts of tetravalent vanadium ion standard solution (prepared by 4mol/L hydrochloric acid) of IL are respectively added, the tetravalent vanadium ion concentration is measured according to the detection method of example 4, each sample is measured for 3 times, the average value is taken, and the standard adding recovery rate is calculated: (labeled sample measurement value-sample measurement value)/(labeled amount×100), and the results are shown in table 3.
TABLE 3 Table 3
As can be seen from Table 3, the method provided by the invention has a labeling recovery rate of 91-105%, which indicates that the method provided by the invention is feasible and has high accuracy.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (7)
1. A method for determining the tetravalent vanadium content in the pickle liquor of a waste denitration catalyst, which is characterized by comprising the following steps:
(1) Scanning all wave lengths of tetravalent vanadium standard solutions with different concentrations to obtain a spectrogram H1, scanning all wave lengths of an acid solution to obtain a spectrogram H2, taking the spectrogram H2 as a reference, differentiating the spectrogram H1 and the spectrogram H2 to obtain a spectrogram H3, and calculating lambda in the spectrogram H3 0 -λ 1 nm to lambda 0 +λ 1 Fitting the nm wavelength band to obtainThe peak area of the obtained peak is used for obtaining a standard peak area S0, and then a standard curve is drawn according to the relation between the concentration of the tetravalent vanadium standard solution and the standard peak area S0;
(2) Pickling the waste denitration catalyst with a soaking solution, performing full-wavelength scanning on the obtained pickling solution to obtain a spectrogram P1, performing full-wavelength scanning on the soaking solution to obtain a spectrogram P2, taking the spectrogram P2 as a reference, performing difference on the spectrogram P1 and the spectrogram P2 to obtain a spectrogram P3, and calculating lambda in the spectrogram P3 0 -λ 1 nm to lambda 0 +λ 1 Fitting the peak area of the obtained peak in the nm wavelength band to obtain a peak area P0, and determining the tetravalent vanadium content in the pickle liquor according to the peak area P0 and a standard curve;
wherein lambda is 0 595-605 nm, lambda 1 45-55 nm, and the scanning wavelength range is 400-1000 nm.
2. The method according to claim 1, wherein in the step (1), the preparation process of the tetravalent vanadium standard solution comprises: and mixing the acid solution with the pH value of 2-6 with vanadyl sulfate.
3. The method of claim 2, wherein in step (1), the acid solution is a dilute sulfuric acid solution.
4. The method according to claim 2, wherein the added amount of vanadyl sulfate is 0.5-20 times of the total mass of vanadium element in the pickle liquor.
5. The method of claim 1, wherein in step (2), the vanadium content of the spent denitration catalyst is not less than 0.2wt%.
6. The method according to claim 1, wherein in step (2), the total vanadium content in the pickling solution is not less than 0.01mg/L.
7. The method according to claim 1, wherein in the step (2), the soaking liquid used for the acid leaching is one or more selected from oxalic acid, nitric acid, hydrochloric acid and citric acid.
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