CN114594064A - Method for testing content of sodium silicate-containing electrolyte - Google Patents

Method for testing content of sodium silicate-containing electrolyte Download PDF

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CN114594064A
CN114594064A CN202210282601.0A CN202210282601A CN114594064A CN 114594064 A CN114594064 A CN 114594064A CN 202210282601 A CN202210282601 A CN 202210282601A CN 114594064 A CN114594064 A CN 114594064A
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reagent
sodium silicate
silicon
solution
molybdenum
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梁伟
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Siberian Motor Technology Suzhou Co ltd
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Siberian Motor Technology Suzhou Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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Abstract

The invention discloses a method for testing the content of sodium silicate-containing electrolyte, which is characterized by comprising the following steps of: acidifying the sodium silicate-containing electrolyte, and then adding an ammonium molybdate reagent to generate a silicon molybdenum yellow reagent; adding reducing substances into the silicon-molybdenum yellow test solution to generate a silicon-molybdenum blue reagent; the reducing substance is ferrous sulfate solution; preparing a standard solution of the content of effective silicon dioxide by using a standard reagent-grade pure sodium silicate solution, and establishing a curve; carrying out absorbance test on the silicon molybdenum blue reagent; the unknown electrolyte sodium silicate concentration is measured according to the principle that different sodium silicate contents in a certain concentration range are in direct proportion to absorbance (according to the beer-Lambert law). The method can improve the testing precision; the method is simple to operate, facilitates batch testing, can be applied to production lines for timing detection, and improves working efficiency.

Description

Method for testing content of sodium silicate-containing electrolyte
Technical Field
The invention relates to the field of electrolyte content testing, in particular to a method for testing the content of sodium silicate electrolyte.
Background
The method for testing the sodium silicate in the electrolyte by using the sodium silicate-containing electrolyte to generate silicic acid precipitate by using hydrochloric acid and silicate radicals and then decomposing the silicic acid precipitate at a certain temperature to generate the silicon dioxide is carried out by using the method, for example, CN102426217A and CN 102393345A.
The sodium silicate-containing electrolyte is tested by adopting a method of adding excessive sodium fluoride in GB/T4209-2008, then adopting methyl red as an indicator, titrating the endpoint with hydrochloric acid and then adopting a sodium hydroxide standard solution back titration method, and the testing precision is not high because the color of the titration endpoint is not easy to judge, certain errors are easy to cause.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the technical problem to be solved by the present invention is how to determine the sodium silicate content of an electrolyte containing sodium silicate with simple steps.
In order to achieve the purpose, the invention provides a content testing method of sodium silicate-containing electrolyte, which is characterized by comprising the following steps of:
1) acidifying the sodium silicate-containing electrolyte, and then adding an ammonium molybdate reagent to generate a silicon molybdenum yellow reagent;
2) adding reducing substances into the silicon-molybdenum yellow test solution to generate a silicon-molybdenum blue reagent; the reducing substance is ferrous sulfate solution;
3) preparing three groups of standard solutions with effective silicon dioxide contents of 3g/L, 5g/L and 7g/L by using a standard reagent grade purity sodium silicate solution, and establishing a curve;
4) carrying out absorbance test on the silicon molybdenum blue reagent;
5) the unknown electrolyte sodium silicate concentration is measured according to the principle that different sodium silicate contents in a certain concentration range are in direct proportion to absorbance (according to the beer-Lambert law).
Further, the step 1) also comprises adding a sulfuric acid reagent for acidification.
Further, the step 1) also comprises the step of adding 1-20 ml of 0.1-2 mol/L sulfuric acid reagent to acidify the mixed electrolyte of sodium silicate and potassium hydroxide, so that a good foundation is formed for generating a stable silicon molybdenum yellow reagent.
Further, an ethanol reagent was added.
Further, 1-20 ml of 10-100% (volume fraction) ethanol reagent is added into the solution formed in the step, so that the color development (absorbance) of the next generated silicon-molybdenum blue reagent is stable.
Further, an ammonium molybdate solution is added to the solution formed in the above step.
Further, 1-15% (mass fraction) of ammonium molybdate solution is added into the solution formed in the step, and the solution is developed for 1-60 min to generate the silicon-molybdenum-yellow reagent.
Further, the step 2) comprises adding 1-15% (mass fraction) of ferrous sulfate, and developing for 30-90 min to generate the silicon-molybdenum blue reagent.
The method disclosed by the invention adopts the steps that ammonium molybdate is added into the acidified electrolyte to generate silicon-molybdenum yellow, then reducing substances are added to reduce the silicon-molybdenum yellow into silicon-molybdenum blue, and the silicate content in the electrolyte is tested by a spectrophotometry method, so that the test precision can be improved; the method is simple to operate, is convenient for batch testing, and can be applied to timing detection on a production line; in addition, the method does not need to add fluorine ions harmful to the environment, greatly reduces the harm to the environment and is beneficial to environmental protection; the method needs a certain time between the two processes of forming the silicon-molybdenum yellow and the silicon-molybdenum blue, the optimal time for forming the silicon-molybdenum yellow is about 30 minutes, and the optimal time for forming the silicon-molybdenum blue is about 1 hour, and the time can be used for processing other matters, so that the working efficiency is improved.
Drawings
FIG. 1 is a standard graph of silica content.
Detailed Description
The technical contents of the preferred embodiments of the present invention will be more clearly and easily understood by referring to the drawings attached to the specification. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
In the drawings, structurally identical elements are represented by like reference numerals, and structurally or functionally similar elements are represented by like reference numerals throughout the several views. The size and thickness of each component shown in the drawings are arbitrarily illustrated, and the present invention is not limited to the size and thickness of each component. The thickness of the components may be exaggerated where appropriate in the figures to improve clarity.
The invention discloses a method for testing the content of sodium silicate electrolyte, which comprises the following steps:
1) acidifying the sodium silicate-containing electrolyte, and then adding an ammonium molybdate reagent to generate a silicon molybdenum yellow reagent;
2) adding reducing substances into the silicon-molybdenum yellow test solution to generate a silicon-molybdenum blue reagent; the reducing substance is ferrous sulfate solution;
3) preparing three groups of standard solutions with effective silicon dioxide contents of 3g/L, 5g/L and 7g/L by using a standard reagent grade purity sodium silicate solution, and establishing a curve;
4) carrying out absorbance test on the silicon-molybdenum-blue reagent;
5) the unknown electrolyte sodium silicate concentration is measured according to the principle that different sodium silicate contents in a certain concentration range are in direct proportion to absorbance (according to the beer-Lambert law).
Preferably, step 1) further comprises acidification by addition of a sulfuric acid reagent.
Preferably, the step 1) further comprises the step of adding 1-20 ml of 0.1-2 mol/L sulfuric acid reagent to acidify the mixed electrolyte of sodium silicate and potassium hydroxide, so as to form a good foundation for generating a stable silicon molybdenum yellow reagent.
Preferably, an ethanol reagent is added.
Preferably, 1-20 ml of 10-100% (volume fraction) ethanol reagent is added into the solution formed in the above step, so that the color development (absorbance) of the next generated "silicon molybdenum blue" reagent is stable.
Preferably, an ammonium molybdate solution is added to the solution formed in the above step.
Preferably, 1-15% (mass fraction) of ammonium molybdate solution is added into the solution formed in the step, and the solution is developed for 1-60 min to generate the silicon-molybdenum-yellow reagent.
Preferably, the step 2) comprises adding 1-15% (mass fraction) of ferrous sulfate, and developing for 30-90 min to generate the silicon-molybdenum-blue reagent.
Another preferred embodiment of the present invention is:
6.1 adding a certain amount of sulfuric acid reagent with certain concentration for acidification:
adding 1-20 ml of 0.1-2 mol/L sulfuric acid reagent to acidify the mixed electrolyte of sodium silicate and potassium hydroxide, and forming a good foundation for generating a stable silicon molybdenum yellow reagent; the sulfuric acid solution with enough amount can inhibit 'silicomolybdic yellow', namely the hybridization of silicomolybdic heteropoly acid, keep the stability of the silicomolybdic heteropoly acid and avoid the interference caused by fluctuation;
6.2 adding a certain amount of ethanol reagent with certain concentration: the addition of the ethanol solution can keep the stability of the absorbance of the silicon molybdenum blue for a long time (not less than 1 hour), and can also improve the test stability of the silicon molybdenum blue;
adding 1-20 ml of 10-100% (volume fraction) ethanol reagent into the solution formed in the step 6.1, so that the color development (absorbance) stability of the next generated silicon-molybdenum-blue reagent can be ensured;
6.3 adding a certain amount of ammonium molybdate solution with certain concentration:
adding 1-15% (mass fraction) of ammonium molybdate solution into the solution formed in the step 6.2, and developing for 1-60 min to generate a silicon-molybdenum-yellow reagent;
6.4 adding a certain amount of ferrous sulfate solution with certain concentration: the reducibility of the ferrous sulfate solution is lower than that of stannous chloride, so that the interference test of a complex compound with a large amount of ammonium molybdate reduced to blue is avoided;
adding 1-15% (mass fraction) ferrous sulfate solution into the solution formed in the step 6.3, and developing for 30-90 min to generate a silicon-molybdenum blue reagent;
6.5 preparing a series of concentration standard solutions by the method (6.1-6.4):
three groups of standard solutions with effective silicon dioxide contents of 3g/L, 5g/L and 7g/L are prepared by using a standard reagent grade pure sodium silicate solution, and a curve (the concentration range is applicable to 1 g/L-20 g/L) is established, wherein the standard curve is shown in figure 1.
6.6 according to the principle that different sodium silicate contents in a certain concentration range are in direct proportion to absorbance (according to the beer-Lambert law), the concentration of the unknown electrolyte sodium silicate is measured.
The calculation principle is as follows: mathematical expression a = lg (1/T) = Kbc according to beer-lambert law
A is the absorbance, T is the transmittance, which is the intensity of incident light in the transmitted light intensity ratio, and K is the molar absorption coefficient, which is related to the nature of the absorbing species and the wavelength λ of the incident light. c is the concentration of the light-absorbing species and b is the thickness of the absorbing layer. The dimension of a container, namely a cuvette, for containing the absorbance of the test liquid, which is placed in the ultraviolet-visible spectrophotometer, is fixed, and the thickness of the absorption layer is the absorption thickness.
A cuvette with a fixed wavelength lambda and a certain size is used, namely lambda and b become constants, the system carries out linear fitting according to input standard liquid with known concentration and corresponding absorbance to obtain a value of K, and then any unknown solution concentration in the concentration range of the standard liquid is calculated.
If three groups of standard solutions C1, C2 and C3 with known concentrations are tested, the absorbance of the standard solutions is A1, A2 and A3 respectively, the K value can be calculated according to the equation A = Kbc of the beer-Lambert law (b is a constant), then an unknown Cx solution to be tested is input, the absorbance of the unknown Cx solution to be tested is measured, and the unknown Cx solution is substituted into the equation to calculate the concentration.
Testing by using an ultraviolet-visible spectrophotometer: the ultraviolet-visible spectrophotometry is a method for determining the absorbance of a substance within the wavelength range of 190-800 nm, and is used for identification, impurity inspection and quantitative determination. When light passes through a solution of a substance to be measured, the degree of absorption of the light by the substance varies depending on the wavelength of the light. The absorption spectrum of a substance has characteristics related to its structure. Thus, a substance can be identified by the ratio of the absorption of the spectrum of the sample to the spectrum of the control over a particular wavelength range. When the method is used for quantification, the absorbance of a sample solution with a certain concentration is measured at the maximum absorption wavelength, and is compared with the absorbance of a control solution with a certain concentration or the concentration of the sample solution is calculated by adopting an absorption coefficient method. The absorbance of the electrolyte with unknown concentration is 0.661Abs, and the concentration of the electrolyte under the absorbance can be automatically obtained by the ultraviolet-visible spectrophotometer according to the linear fitting function of the curve.
The method is suitable for testing the content of sodium silicate in the electrolyte without containing silicon, selenium, arsenic and other anions.
The method disclosed by the invention adopts the steps that ammonium molybdate is added into the acidified electrolyte to generate silicon-molybdenum yellow, then reducing substances are added to reduce the silicon-molybdenum yellow into silicon-molybdenum blue, and the silicate content in the electrolyte is tested by a spectrophotometry method, so that the test precision can be improved; the method is simple to operate, is convenient for batch testing, and can be applied to timing detection on a production line; in addition, fluorine ions harmful to the environment are not added in the method, so that the harm to the environment is greatly reduced, and the method is beneficial to environmental protection; the method needs a certain time between the two processes of forming the silicon-molybdenum yellow and the silicon-molybdenum blue, the optimal time for forming the silicon-molybdenum yellow is about 30 minutes, and the optimal time for forming the silicon-molybdenum blue is about 1 hour, and other matters can be processed by utilizing the time, so that the working efficiency is improved.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions that can be obtained by a person skilled in the art through logical analysis, reasoning or limited experiments based on the prior art according to the concepts of the present invention should be within the scope of protection determined by the claims.

Claims (8)

1. The method for testing the content of the sodium silicate-containing electrolyte is characterized by comprising the following steps of:
1) acidifying the sodium silicate-containing electrolyte, and then adding an ammonium molybdate reagent to generate a silicon molybdenum yellow reagent;
2) adding reducing substances into the silicon-molybdenum yellow test solution to generate a silicon-molybdenum blue reagent; the reducing substance is ferrous sulfate solution;
3) preparing three groups of standard solutions with effective silicon dioxide contents of 3g/L, 5g/L and 7g/L by using a standard reagent grade sodium silicate solution, and establishing a curve;
4) carrying out absorbance test on the silicon molybdenum blue reagent;
5) the unknown electrolyte sodium silicate concentration is measured according to the principle that different sodium silicate contents in a certain concentration range are in direct proportion to absorbance (according to the beer-Lambert law).
2. The method of claim 1, wherein step 1) further comprises acidification by the addition of a sulfuric acid reagent.
3. The method as claimed in claim 2, wherein the step 1) further comprises adding 1-20 ml of 0.1-2 mol/L sulfuric acid reagent to acidify the mixed electrolyte of sodium silicate and potassium hydroxide, so as to form a base for generating stable 'silicomolybdic yellow' reagent.
4. The method of claim 2, wherein an ethanol reagent is added.
5. The method of claim 3, wherein 1-20 ml of 10-100% (volume fraction) ethanol reagent is added to the solution formed in the above step, so that the subsequent color development (absorbance) of the generated "silicon molybdenum blue" reagent is stable.
6. The method of claim 4 wherein an ammonium molybdate solution is added to the solution formed in said step.
7. The method of claim 5, wherein 1% to 15% (mass fraction) of ammonium molybdate solution is added to the solution formed in the above step, and the solution is developed for 1 to 60min to generate the reagent "silicomolybdic yellow".
8. The method as claimed in claim 1, wherein the step 2) comprises adding 1% to 15% (mass fraction) of ferrous sulfate, and developing for 30 to 90min to generate the reagent "silicon molybdenum blue".
CN202210282601.0A 2022-03-22 2022-03-22 Method for testing content of sodium silicate-containing electrolyte Pending CN114594064A (en)

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