CN113820445B - Method for detecting concentration of cold rolling circulation leveling liquid - Google Patents

Method for detecting concentration of cold rolling circulation leveling liquid Download PDF

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CN113820445B
CN113820445B CN202010557871.9A CN202010557871A CN113820445B CN 113820445 B CN113820445 B CN 113820445B CN 202010557871 A CN202010557871 A CN 202010557871A CN 113820445 B CN113820445 B CN 113820445B
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瞿培磊
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Baoshan Iron and Steel Co Ltd
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Abstract

The invention discloses a method for detecting the concentration of cold rolling circulating leveling liquid, which adopts acid-base titration to respectively detect the content of acidic substances and alkaline substances in leveling stock solution and leveling liquid to be detected, and calculates the concentration of the leveling liquid to be detected through a formula. According to the method for detecting the concentration of the cold rolling circulation leveling liquid, disclosed by the invention, the acid-base property of chemical substances added into the leveling liquid can be utilized to effectively detect the cold rolling circulation leveling liquid used in the cold rolling production process, so that the more accurate concentration of the leveling liquid is obtained.

Description

Method for detecting concentration of cold rolling circulation leveling liquid
Technical Field
The invention relates to the field of concentration detection of flattening liquid, in particular to a method for detecting concentration of flattening liquid in a cold rolling cycle.
Background
Modern steel production is usually equipped with a cold rolling leveling procedure, wherein leveling refers to processing under slight thinning pressure through leveling equipment after recrystallization annealing of cold-rolled strip steel, so that a material yield platform after recrystallization annealing disappears, the flatness of the strip steel is improved, and the surface quality of high-quality strip steel with uniform quality is obtained; in the process of modern cold rolling production, most of the production is assisted by adopting a leveling liquid, wherein the leveling liquid is a chemical substance used for producing by spraying a chemical leveling liquid substance and water into strip steel and rollers of a leveling machine according to a certain proportion; the leveling liquid generally plays a plurality of roles in production, mainly lubrication, cleaning and rust prevention; because the leveling liquid has excellent performance and multiple functions, most leveling units use the leveling liquid in the production line of modern iron and steel enterprises, and in the existing leveling liquid units, the leveling liquid is used once, namely, a certain amount of leveling stock solution is mixed with water and then sprayed onto strip steel and rollers for use, and then the leveling liquid is collected and treated as wastewater, so that the production process management can be simplified to the greatest extent and the product quality of the production process can be ensured, but a large amount of chemical wastewater is discharged all the time in the production process, and therefore, the iron and steel enterprises are researching the use process of the circulating leveling liquid; therefore, in this process, the concentration detection technology of the circulating leveling liquid is an urgent technical problem.
In the existing leveling machine set, a simple sugar meter is used for detecting the concentration of the leveling liquid, or in actual production, a mass flowmeter is used for preparing the needed leveling liquid without detecting the concentration, the concentration is measured by utilizing the change of refractive indexes generated in the leveling liquid with different concentrations by light, but once the leveling liquid is changed to be circulated, dirt in the whole rolling process is gradually accumulated in the leveling liquid to change the refractive index, and the leveling liquid is gradually consumed in the circulation process; so that the traditional concentration monitoring method fails; the technical problem of detecting the concentration of the cold rolling leveling liquid is mainly that the leveling liquid is a special chemical substance, unlike common oily metal processing liquid, the metal processing liquid is processing oil and is not or slightly soluble in water, and the leveling liquid is a substance only soluble in water, so that the traditional heating or oil phase detection and analysis means cannot be used; however, after the whole leveling liquid is subjected to a circulating process, a lack of concentration detection technology will bring about a non-negligible problem to production operation, so that development of corresponding technology is urgently required.
Based on the above, technical data and patent documents related to concentration detection of leveling liquid and water-soluble metal liquid have been searched in the art, and are mainly focused in the following documents: application number 201010213754.7 discloses a leveling liquid concentration control system and method, which adopts a leveling liquid concentration control technology in an online production process, mainly utilizes the total flow of leveling liquid and water in unit time to prepare leveling liquid with various concentrations through a flowmeter, and the method can only be used for preparing the concentration of the leveling liquid, but cannot analyze and detect the prepared concentration of the leveling liquid, and has very limited application occasions. Application number 201710596741.4 discloses an automatic leveling liquid preparation method based on online conductivity measurement, wherein the online concentration detection method is provided, the online leveling liquid conductivity meter is installed for measurement, the real-time concentration of the leveling liquid is fitted by utilizing the relation between different concentrations and conductivities, the method is applicable to the traditional leveling liquid, but various pollutants gradually appear after the leveling liquid is recycled, at the moment, the conductivities measured by the method can be greatly influenced by the pollutants, the accurate concentration can not be accurately measured, and therefore the method is difficult to use. Application number 201711118946.8 discloses a cutting fluid concentration test method, which comprises the steps of preparing liquid standard samples with different concentrations by using original cutting fluid and water with different volumes, measuring refractive indexes at different concentrations, and comparing the refractive indexes of the cutting fluid in a working state with the difference of the standard samples to obtain an actual concentration value; the method can be suitable for cutting fluid, but for the working state of leveling fluid, a large amount of iron powder, hydraulic oil, dirt and other substances are contained in the leveling fluid, the refractive index change is extremely large, and the detection by the method is difficult. The application number 201811378664.6 discloses a method, a device and a system for monitoring the concentration of cutting fluid, and provides another method for monitoring the concentration of the cutting fluid, and the main principle is that the concentration of the fitting leveling fluid is measured by utilizing the specific gravity of the cutting fluid to be tested, and the concentration of the leveling fluid in the cold rolling production process is generally lower and is only in the vicinity of 1-5%, so that most of the leveling fluid is water, the specific gravity of the leveling fluid with different concentrations is not changed greatly, and the concentration detection by utilizing the method can generate a great error. Application No. 201821914084.X discloses a glass grinding fluid concentration detection device, which uses a plurality of filtering membranes and active carbon filtering membranes to filter impurities in the grinding fluid and then performs optical refractive index measurement; if the method is used for measuring the concentration of the leveling liquid, although the influence of various impurities in field production can be reduced, a great amount of effective chemical substances of the leveling liquid can be adsorbed by the use of the filtering membrane, so that the concentration detection result deviates from an actual value.
In view of the above, it is desirable to develop a new method for detecting the concentration of the flattening liquid, which can effectively detect the flattening liquid of the cold rolling cycle used in the production process, and has high accuracy.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for detecting the concentration of cold rolling circulating leveling liquid, which can effectively detect the cold rolling circulating leveling liquid used in the cold rolling production process by utilizing the acid-base property of chemical substances added in the leveling liquid, so as to obtain the accurate concentration of the leveling liquid.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the method for detecting the concentration of the cold rolling circulating leveling liquid comprises the steps of respectively measuring the consumption of acid and alkali in the stock leveling liquid diluent and the to-be-measured leveling liquid diluent by acid-alkali titration to obtain the concentration of acidic substances and the concentration of alkaline substances in the to-be-measured leveling liquid, thereby obtaining the concentration of the to-be-measured leveling liquid.
Preferably, the method for detecting the concentration of the cold rolling circulation leveling liquid comprises the following steps:
s1, preparing a flattening stock solution diluent and a flattening stock solution diluent to be tested respectively, then titrating the flattening stock solution diluent and the flattening stock solution diluent to be tested respectively by using hydrochloric acid until the pH value becomes 4+/-0.05, measuring the consumption of the hydrochloric acid in the flattening stock solution diluent and the flattening stock solution diluent to be tested, and calculating to obtain the concentration of alkaline substances in the flattening stock solution to be tested;
s2, respectively preparing a diluent of the leveling stock solution and a diluent of the leveling solution to be measured, then respectively titrating the diluent of the leveling stock solution and the diluent of the leveling solution to be measured by using a potassium hydroxide solution until the pH value becomes 11+/-0.05, measuring the consumption of potassium hydroxide in the diluent of the leveling stock solution and the diluent of the leveling solution to be measured, and calculating the concentration of acidic substances in the leveling solution to be measured;
s3, obtaining the concentration of the leveling liquid to be measured through the concentration of the alkaline substance and the concentration of the acidic substance in the leveling liquid to be measured.
Preferably, the step S1 specifically includes the following steps:
s11, weighing m p1 Placing 1-5 g of flattening stock solution into a standard beaker, and preparing 150ml of flattening stock solution diluent by deionized water; titration with hydrochloric acid until pH became 4.+ -. 0.05 was carried out, and the total volume consumed by hydrochloric acid was recorded as H p1
S12, weighing m u1 Placing the to-be-measured leveling liquid with the concentration of between 20 and 50g in a standard beaker, and preparing 150ml of to-be-measured leveling liquid diluent by deionized water; titration with hydrochloric acid until pH became 4.+ -. 0.05 was carried out, and the total volume consumed by hydrochloric acid was recorded as H u1
S13, the concentration of alkaline substances in the leveling liquid to be measured is calculated as mass fraction C 1 The concentration of alkaline substances in the leveling liquid to be measured is calculated by the following formula:
wherein C is 1 : concentration of alkaline substances in the leveling liquid to be measured,%;
H p1 : in the step S11, when the pH value is changed to 4+/-0.05 by titration with hydrochloric acid, the total volume of hydrochloric acid consumed by the stock solution diluent is leveled, and ml is leveled;
H u1 : in the step S12, when the pH value is changed to 4+/-0.05, the total volume of hydrochloric acid consumed by the diluent of the leveling liquid to be tested is ml;
m p1 : in the step S11, the mass of the weighed leveling stock solution, g;
m u1 : in step S12, the mass, g, of the leveling liquid to be measured is weighed.
Preferably, the step S2 specifically includes the following steps:
s21, weighing m p2 Placing 1-5 g of flattening stock solution into a standard beaker, adding 5-20 g of glycerol reagent, preparing 150ml of flattening stock solution diluent by deionized water, and stirring for at least 20min; titration with potassium hydroxide solution until pH became 11.+ -. 0.05, the total volume consumed by potassium hydroxide was recorded as H p2
S22, weighing m u2 Placing 20-50 g of to-be-measured leveling liquid into a standard beaker, adding 5-10 g of glycerol reagent, preparing 150ml of to-be-measured leveling liquid diluent by deionized water, and stirring for at least 20min; titration with potassium hydroxide solution until pH became 11.+ -. 0.05, the total volume consumed by potassium hydroxide was recorded as H u2
S23, the concentration of acidic substances in the leveling liquid to be measured is calculated as mass fraction C 2 The concentration of acidic substances in the leveling liquid to be measured is calculated by the following formula:
wherein C is 2 : concentration of acidic substances in the leveling liquid to be measured,%;
H p2 : in the step S21, when the pH value is changed to 11+/-0.05, the total volume of potassium hydroxide consumed by the stock solution diluent is leveled, and ml is obtained;
H u2 : in the step S22, when the pH value is changed to 11+/-0.05, the total volume of the consumed potassium hydroxide in the diluent of the leveling liquid to be tested is ml;
m p2 : in the step S21, the mass of the weighed leveling stock solution, g;
m u2 : in step S22, the mass, g, of the leveling liquid to be measured is weighed.
Preferably, in the step S3, the concentration of the leveling liquid to be measured is calculated as a mass fraction C TPL The concentration of the leveling liquid to be measured is calculated using the formula:
C TPL =[A·C 1 +(1-A)·C 2 ]·100%
wherein C is TPL : concentration of the leveling liquid to be measured,%;
a: the concentration influence coefficient is less than or equal to 1 and is a dimensionless value;
C 1 : concentration of alkaline substances in the leveling liquid to be measured,%;
C 2 : acidic material in leveling liquid to be measuredConcentration,%.
Preferably, in the step S11 and the step S12, the concentration of the hydrochloric acid is 0.005 to 0.1mol/l.
Preferably, in the step S11, the stock solution diluent is configured and titrated under the constant temperature condition of 20-25 ℃;
preferably, in the step S12, the diluent of the leveling liquid to be tested is configured and titrated under the constant temperature condition of 20-25 ℃.
Preferably, in the step S21 and the step S22, the concentration of the potassium hydroxide solution is 0.02 to 0.6mol/l.
Preferably, in the step S21, the stock solution diluent is configured and titrated under the constant temperature condition of 30-55 ℃;
in the step S22, the diluent of the leveling liquid to be tested is configured and titrated under the constant temperature condition of 30-55 ℃.
Preferably, in the step S5, the concentration influence coefficient a is 0.5 to 1.
Preferably, the concentration influence coefficient a is 0.5 to 0.6.
The method for detecting the concentration of the cold rolling circulation leveling liquid is based on the following principle: in the production process of the cold rolling circulation leveling liquid, along with the circulation and repeated use of the leveling liquid, various chemical reagents can react, volatilize and adsorb strip steel at any time to be consumed and reduced, and the consumption rates of various chemical substances in the leveling liquid are different, for example, the concentration is measured according to the total sum of the chemical substances of the whole leveling liquid in the traditional sense, namely, the actual production condition change cannot be displayed due to difficult operation. It is therefore generally more reasonable to define the concentration of the levelling liquid in the circulation process to follow the production requirements of the unit process, i.e. to monitor the change in the content of chemical substances which play a critical role in a certain class of functions as a whole concentration of the circulated levelling liquid, depending on the equipment production and the core requirements of the product.
The main chemical substances in the leveling liquid are detected through gas chromatography-mass spectrometry chemical analysis performed by using common typical leveling liquid in some production, and the main chemical substances of the leveling liquid can be known to be mainly the following substances through comparison of standard spectrograms: benzene, ethanolamine, 1-amino-2-propanol, D-aminopropanol, monoethanolamine, diethanolamine, triethanolamine, 2-methyl octanoic acid, nonanoic acid, dodecanedioic acid, decaethylene glycol and the like, and further summarizing, it is known that the leveling liquid mainly contains more alkaline substances (such as alcohol amine and the like) and acidic substances (such as organic acids) and a small amount of alcohols and aromatic compounds. Among them, the alcohol amine compound and the organic acid compound are main substances for rust prevention and lubrication of the leveling process, the former is generally high in alkalinity, and the latter is weak in acidity, and the two are the most important chemical reagents in the leveling liquid. Thus, with the chemical basicity of the former, when the solution is dropped with an acid (e.g., hydrochloric acid) or the like, the acid can react with the basic substance in the leveling solution, such as with an ethanolamine substance, as follows:
N(CH 2 CH 2 OH)n+HCl=[HN(CH 2 CH 2 OH)n]Cl
meanwhile, titration is performed by using chemical alkali (such as potassium hydroxide) or the like, and the alkali can react with acidic substances (organic acid substances) in the leveling liquid, such as reaction with chemical organic acid:
R-COOH+KOH=R-COOK+H 2 O
therefore, considering that the acid-base substance is a reagent playing a core role in the leveling liquid, the consumption of the substance in the circulation process can be obtained by adopting a titration method, and the concentration of the circulation leveling liquid can be accurately calculated by comparing the consumption with the unused leveling liquid.
It should be noted that there is also a difference in actual consumption rate due to various alkaline substances and acidic substances contained in the leveler liquid. Therefore, in the calculation of the concentration, the concentration of the circulating liquid can be defined by considering the importance requirements of different units on the acid-base substances in production. In the method, hydrochloric acid titration pH is changed to 4+/-0.05 as an endpoint calculation criterion of alkaline substance titration, and potassium hydroxide titration pH is changed to 11+/-0.05 as an endpoint calculation criterion of acidic substance titration.
The beneficial effects of the invention are as follows:
according to the method for detecting the concentration of the cold rolling circulating leveling liquid, the property of the cold rolling leveling liquid is fully considered, the acid-base property of chemical substances is added into the leveling liquid, and the acid-base titration treatment is carried out on the stock solution of the leveling liquid and the cold rolling circulating leveling liquid used in the cold rolling production process, so that the accurate concentration of the leveling liquid is obtained; the method has the advantages of simple operation process, rapid detection result, wide practical prospect and high detection precision.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way.
According to the method for detecting the concentration of the cold rolling circulating leveling liquid, provided by the invention, the consumption of the leveling stock solution diluent and the consumption of the acid and the alkali in the leveling liquid diluent to be detected are respectively measured through acid-base titration, so that the concentration of the acidic substance and the concentration of the alkaline substance in the leveling liquid to be detected are obtained, and the concentration of the leveling liquid to be detected is obtained; the principle is that an acid-base titration method is adopted to respectively measure the consumption of acid and alkali in unused stock solution diluent and the diluent of the to-be-measured leveling solution, and then the actual amounts of alkaline substances (such as alcohol amine substances and the like) and acidic substances (such as organic acid substances and the like) in the to-be-measured leveling solution are calculated through comparison. Meanwhile, because the composition difference of the leveling liquid in the actual production process is large, the actual consumption of alkaline substances and acidic substances can be different to a certain extent. Therefore, according to the importance of the two to production and the actual titration measurement result, the concentration of the leveling liquid to be measured is comprehensively calculated by combining the process requirements of the leveling liquid production.
The method for detecting the concentration of the cold rolling circulation leveling liquid comprises the following steps:
s1, preparing a flattening stock solution diluent and a flattening stock solution diluent to be tested respectively, then titrating the flattening stock solution diluent and the flattening stock solution diluent to be tested respectively by using hydrochloric acid until the pH value becomes 4+/-0.05, obtaining the consumption of the hydrochloric acid in the flattening stock solution diluent and the flattening stock solution diluent to be tested, and obtaining the concentration of alkaline substances in the flattening stock solution to be tested through calculation;
the step S1 specifically comprises the following steps:
s11, weighing m p1 Placing 1-5 g of flattening stock solution into a 250ml standard beaker, and preparing 150ml of flattening stock solution diluent by deionized water under the constant temperature condition of 20-25 ℃; placing a pH detector into the flattening stock solution, slowly adding 0.005-0.1 mol/l hydrochloric acid dropwise under stirring at a constant temperature of 20-25 ℃ for titration until the pH becomes 4+/-0.05, and recording that the total volume consumed by the hydrochloric acid is H p1
S12, weighing m u1 Placing the to-be-measured leveling liquid with the concentration of between 20 and 50g in a standard beaker with the concentration of 250ml, and preparing 150ml of to-be-measured leveling liquid diluent with deionized water under the constant temperature condition with the temperature of between 20 and 25 ℃; placing a pH detector into a diluent of a leveling liquid to be detected, slowly adding 0.005-0.1 mol/l hydrochloric acid dropwise under stirring at a constant temperature of 20-25 ℃ for titration until the pH becomes 4+/-0.05, and recording that the total volume consumed by the hydrochloric acid is H u1
S13, the concentration of alkaline substances in the leveling liquid to be measured is calculated as mass fraction C 1 The concentration of alkaline substances in the leveling liquid to be measured is calculated by the following formula:
wherein C is 1 : concentration of alkaline substances in the leveling liquid to be measured,%;
H p1 : in the step S11, when the pH value is changed to 4+/-0.05 by titration with hydrochloric acid, the total volume of hydrochloric acid consumed by the stock solution diluent is leveled, and ml is leveled;
H u1 : in the step S12, when the pH value is changed to 4+/-0.05, the total volume of hydrochloric acid consumed by the diluent of the leveling liquid to be tested is ml;
m p1 : in the step S11, the mass of the weighed leveling stock solution, g;
m u1 : in step S12, the mass, g, of the leveling liquid to be measured is weighed.
In the process, hydrochloric acid fully reacts with alkaline substances (alcohol amine substances such as most of monoethanolamine, diethanolamine, triethanolamine and the like) in the stock solution diluent and the to-be-measured leveling solution diluent in the process that the titration pH value is changed to 4+/-0.05; the concentration of alkaline substances in the diluted solution of the leveling stock solution and the diluted solution of the leveling solution to be measured can be calculated through the consumption of hydrochloric acid with corresponding concentration;
s2, respectively preparing a diluent of the leveling stock solution and a diluent of the leveling solution to be measured, then respectively titrating the diluent of the leveling stock solution and the diluent of the leveling solution to be measured by using a potassium hydroxide solution until the pH value becomes 11+/-0.05, obtaining the diluent of the leveling stock solution and the consumption of potassium hydroxide in the diluent of the leveling solution to be measured, and obtaining the concentration of acidic substances in the leveling solution to be measured through calculation;
the step S2 specifically includes the following steps:
s21, weighing m p2 Placing 1-5 g of flattening stock solution into a 250ml standard beaker, adding 5-20 g of glycerol reagent under the constant temperature condition of 30-55 ℃, preparing 150ml of flattening stock solution diluent by using deionized water, and keeping the constant temperature and stirring time for at least 20min; the pH detector is placed in the flattening stock solution, under the constant temperature condition of 30-55 ℃ with stirring, 0.02-0.6 mol/l potassium hydroxide solution is slowly added dropwise for titration until the pH becomes 11+/-0.05, and the total volume consumed by potassium hydroxide is recorded as H p2
S22, weighing m u2 Placing 20-50 g of leveling liquid to be tested in a 250ml standard beaker, adding 5-10 g of glycerol reagent under the constant temperature condition of 30-55 ℃, preparing 150ml of leveling liquid diluent to be tested by deionized water, and keeping the constant temperature and stirring time for at least 20min; the pH detector is placed in the diluent of the leveling liquid to be detected, under the constant temperature condition of stirring and 30-55 ℃, 0.02-0.6 mol/l potassium hydroxide solution is slowly added dropwise for titration until the pH value becomes 11+/-0.05, and the total volume consumed by the potassium hydroxide is recorded as H u2
S23, the concentration of acidic substances in the leveling liquid to be measured is calculated as mass fraction C 2 The method is characterized in that the acidic substances in the leveling liquid to be measured are calculated by usingIs the concentration of (1):
wherein C is 2 : concentration of acidic substances in the leveling liquid to be measured,%;
H p2 : in the step S21, when the pH value is changed to 11+/-0.05, the total volume of potassium hydroxide consumed by the stock solution diluent is leveled, and ml is obtained;
H u2 : in the step S22, when the pH value is changed to 11+/-0.05, the total volume of the consumed potassium hydroxide in the diluent of the leveling liquid to be tested is ml;
m p2 : in the step S21, the mass of the weighed leveling stock solution, g;
m u2 : in step S22, the mass, g, of the leveling liquid to be measured is weighed.
In the process, potassium hydroxide fully reacts with acidic substances (organic acid substances) in the stock solution diluent and the to-be-measured flattening solution diluent; the concentration of acidic substances in the stock solution diluent and the to-be-measured stock solution diluent can be calculated through the consumption of potassium hydroxide with corresponding concentration; the method comprises the steps of carrying out a first treatment on the surface of the
S3, obtaining the concentration of the leveling liquid to be measured through the concentration of the alkaline substances and the concentration of the acidic substances in the leveling liquid to be measured;
the concentration of the leveling liquid to be measured is calculated by mass fraction C TPL The concentration of the leveling liquid to be measured is calculated using the formula:
C TPL =[A·C 1 +(1-A)·C 2 ]·100%
wherein C is TPL : concentration of the leveling liquid to be measured,%;
a: the concentration influence coefficient is less than or equal to 1 and is a dimensionless value;
C 1 : concentration of alkaline substances in the leveling liquid to be measured,%;
C 2 : concentration of acidic substances in the leveling liquid to be measured,%.
Wherein the concentration influence coefficient A is 0.5-1, preferably 0.5-0.6, and the concentration influence coefficient A is specifically related to the type of the flattening stock solution.
The method for detecting the concentration of the cold rolling circulation leveling liquid is further described below with reference to specific examples;
example 1
In certain leveling machine equipment on site, the cold rolling leveling liquid of the unit is recovered, and the original proportioning concentration of the leveling liquid before use is 5%.
S1, measuring the concentration of alkaline substances in the leveling liquid
S11, weighing m p1 2.04g of the stock solution for leveling is placed in a standard beaker of 250ml, and 150ml of stock solution for leveling is prepared by deionized water under stirring at a constant temperature of 20 ℃; placing a pH detector in the flattening stock solution, slowly adding 0.0208mol/l hydrochloric acid dropwise under stirring at 20deg.C for titration, continuously recording pH value until the pH value becomes 3.98, and recording total volume consumed by hydrochloric acid as H p1 =76.55ml;
S12, weighing m u1 Placing 25.01g of the leveling liquid to be tested in a standard beaker with 250ml, and preparing 150ml of the leveling liquid to be tested diluent with deionized water under the constant temperature condition of stirring and 20 ℃; placing a pH detector in the diluent of the leveling liquid to be detected, slowly adding 0.0208mol/l hydrochloric acid dropwise under stirring at a constant temperature of 20 ℃ for titration until the pH becomes 4.04, and recording that the total volume consumed by the hydrochloric acid is H u1 =43.72ml;
S13, the concentration of alkaline substances in the leveling liquid to be measured is calculated as mass fraction C 1 The concentration of alkaline substances in the leveling liquid to be measured is calculated by the following formula:
s2, the concentration of acidic substances in the leveling liquid to be measured
S21, weighing m p2 2.18g of the levelling stock solution was placed in a 250ml standard beaker and 5g of glycerol reagent was added at a constant temperature of 45℃for usePreparing 150ml of flat stock solution diluent by using ionized water, and keeping the constant temperature and stirring time for at least 1h; the pH detector is placed in the flattening stock solution, 0.025mol/l potassium hydroxide solution is slowly added dropwise under the constant temperature condition of stirring and 45 ℃ for titration until the pH becomes 11.04, and the total volume consumed by potassium hydroxide is recorded as H p2 =46.86ml;
S22, weighing m u2 Placing 25.33g of leveling liquid to be tested in a 250ml standard beaker, adding 7g of glycerol reagent under the constant temperature condition of 45 ℃, preparing 150ml of leveling liquid diluent to be tested by deionized water, and keeping the constant temperature and stirring time for at least 1h; the pH detector is placed in the diluent of the leveling liquid to be detected, 0.025mol/l potassium hydroxide solution is slowly added dropwise for titration under the constant temperature condition of stirring and 45 ℃, and when the pH value becomes 11.02, the total volume consumed by the potassium hydroxide is recorded as H u2 =28.64ml;
S23, the concentration of acidic substances in the leveling liquid to be measured is calculated as mass fraction C 2 The concentration of acidic substances in the leveling liquid to be measured is calculated by the following formula:
s3, the concentration of the leveling liquid to be measured is calculated by mass fraction C TPL Representing, calculating the concentration of the leveling liquid to be measured by using the following formula, wherein the concentration influence coefficient a=0.6;
C TPL =[A·C 1 +(1-A)·C 2 ]·100%=4.9%
in the concentration detection process of the leveling liquid to be detected, the leveling liquid to be detected samples liquid from field use, and the concentration of 4.9% detected according to the method is less than 5% of the original concentration in consideration of the leveling liquid loss existing in production, but can reflect the actual concentration level of the leveling liquid in a circulating mode more truly.
Example 2
In certain leveling machine equipment on site, the cold rolling leveling liquid of the unit is recovered, and the original proportioning concentration of the leveling liquid before use is 2.5%.
S1, measuring the concentration of alkaline substances in the leveling liquid
S11, weighing m p1 The stock solution with the flatness of 3.47g is placed in a standard beaker with 250ml, and 150ml of stock solution dilution is prepared by deionized water under stirring and at a constant temperature of 20 ℃; placing a pH detector into the flattening stock solution, slowly adding 0.015mol/l hydrochloric acid dropwise under stirring at 20deg.C for titration, continuously recording pH value until pH becomes 4.03, and recording total volume consumed by hydrochloric acid as H p1 =110.47ml;
S12, weighing m u1 Placing 45.04g of the leveling liquid to be tested in a standard beaker with 250ml, and preparing 150ml of the leveling liquid to be tested diluent with deionized water under the constant temperature condition of stirring and 20 ℃; the pH detector is placed in the diluent of the leveling liquid to be detected, 0.015mol/l hydrochloric acid is slowly added dropwise for titration under the constant temperature condition of stirring and 20 ℃, and when the pH value becomes 4.05, the total volume consumed by the hydrochloric acid is recorded as H u1 =35.22ml;
S13, the concentration of alkaline substances in the leveling liquid to be measured is calculated as mass fraction C 1 The concentration of alkaline substances in the leveling liquid to be measured is calculated by the following formula:
s2, the concentration of acidic substances in the leveling liquid to be measured
S21, weighing m p2 Placing 3.88g of flattening stock solution in a 250ml standard beaker, adding 6g of glycerol reagent under the constant temperature condition of 45 ℃, preparing 150ml of flattening stock solution diluent by deionized water, and keeping the constant temperature and stirring for 1h; the pH detector is placed in the flattening stock solution, 0.02mol/l potassium hydroxide solution is slowly added dropwise under the constant temperature condition of stirring and 45 ℃ for titration until the pH value becomes 10.98, and the total volume consumed by potassium hydroxide is recorded as H p2 =110.20ml;
S22, weighing m u2 The leveling liquid to be measured, which is 47.52g, is placed in a standard beaker of 250ml at a temperatureAdding 10g of glycerol reagent under the constant temperature condition with the temperature of 45 ℃, preparing 150ml of to-be-measured leveling liquid diluent by using deionized water, and keeping the constant temperature and stirring time for at least 1h; the pH detector is placed in the diluent of the leveling liquid to be detected, 0.02mol/l potassium hydroxide solution is slowly added dropwise for titration under the constant temperature condition of stirring and 45 ℃ until the pH value becomes 11.04, and the total volume consumed by the potassium hydroxide is recorded as H u2 =36.43ml;
S23, the concentration of acidic substances in the leveling liquid to be measured is calculated as mass fraction C 2 The concentration of acidic substances in the leveling liquid to be measured is calculated by the following formula:
s3, the concentration of the leveling liquid to be measured is calculated by mass fraction C TPL Representing, calculating the concentration of the leveling liquid to be measured by using the following formula, wherein the concentration influence coefficient a=0.65;
C TPL =[A·C 1 +(1-A)·C 2 ]·100%=2.54%
in the concentration detection process of the leveling liquid to be detected, the leveling liquid to be detected samples liquid from field use, and the concentration level of the leveling liquid in actual circulation can be truly reflected according to the concentration of 2.54% detected by the method in consideration of continuous leveling liquid use loss in production and errors in the addition process.
Example 3
In certain leveling machine equipment on site, cold rolling of a recovery unit is leveled, and the original proportioning concentration of the leveling liquid before use is 4.5%.
S1, measuring the concentration of alkaline substances in the leveling liquid
S11, weighing m p1 A stock solution for leveling, which is 1.05g, is placed in a standard beaker of 250ml, and a dilution of 150ml of stock solution for leveling is prepared by deionized water under stirring at a constant temperature of 20 ℃; placing a pH detector in the flattening stock solution, slowly adding 0.005mol/l hydrochloric acid dropwise under stirring at 20deg.C for titration, and continuously recording pH until pH becomesAt 3.95, the total volume of hydrochloric acid consumption was recorded as H p1 =209.82ml;
S12, weighing m u1 Placing the to-be-measured leveling liquid with the concentration of 20.20g in a standard beaker with the concentration of 250ml, and preparing 150ml of to-be-measured leveling liquid diluent with deionized water under the constant temperature condition of stirring and the temperature of 20 ℃; placing a pH detector into the diluent of the leveling liquid to be detected, slowly adding 0.005mol/l hydrochloric acid dropwise under stirring at a constant temperature of 20 ℃ for titration until the pH value becomes 3.96, and recording that the total volume consumed by the hydrochloric acid is H u1 =174.98ml;
S13, the concentration of alkaline substances in the leveling liquid to be measured is calculated as mass fraction C 1 The concentration of alkaline substances in the leveling liquid to be measured is calculated by the following formula:
s2, the concentration of acidic substances in the leveling liquid to be measured
S21, weighing m p2 Placing 1.00g of flattening stock solution into a 250ml standard beaker, adding 5g of glycerol reagent under the constant temperature condition of 45 ℃, preparing 150ml of flattening stock solution diluent by using deionized water, and keeping the constant temperature and stirring for 20min; the pH detector is placed in the flattening stock solution, 0.02mol/l potassium hydroxide solution is slowly added dropwise under the constant temperature condition of stirring and 45 ℃ for titration until the pH value becomes 10.98, and the total volume consumed by potassium hydroxide is recorded as H p2 =25.78ml;
S22, weighing m u2 Placing 20.00g of leveling liquid to be tested in a 250ml standard beaker, adding 5g of glycerol reagent under the constant temperature condition of 45 ℃, preparing 150ml of leveling liquid diluent to be tested by deionized water, and keeping the constant temperature and stirring for 20min; the pH detector is placed in the diluent of the leveling liquid to be detected, 0.02mol/l potassium hydroxide solution is slowly added dropwise for titration under the constant temperature condition of stirring and 45 ℃ until the pH value becomes 10.95, and the total volume consumed by the potassium hydroxide is recorded as H u2 =24.24ml;
S23, waiting forMeasuring the concentration of acidic substances in the leveling liquid to obtain mass fraction C 2 The concentration of acidic substances in the leveling liquid to be measured is calculated by the following formula:
s3, the concentration of the leveling liquid to be measured is calculated by mass fraction C TPL Representing, calculating the concentration of the leveling liquid to be measured by using the following formula, wherein the concentration influence coefficient a=0.5;
C TPL =[A·C 1 +(1-A)·C 2 ]·100%=4.51%
in the concentration detection process of the leveling liquid to be detected, the leveling liquid to be detected samples liquid from field use, and the concentration level of the leveling liquid in actual circulation can be truly reflected according to the concentration of 4.51% detected by the method in consideration of continuous leveling liquid use loss in production and errors in the addition process.
Example 4
In certain leveling machine equipment on site, the concentration of the original proportioning of the cold rolling leveling liquid of the recovery unit is 6 percent before the leveling liquid is used.
S1, measuring the concentration of alkaline substances in the leveling liquid
S11, weighing m p1 A stock solution for leveling, which is =5.00 g, is placed in a standard beaker of 250ml, and a dilution of the stock solution for leveling, which is 150ml, is prepared with deionized water under stirring at a constant temperature of 25 ℃; placing a pH detector into the flattening stock solution, slowly adding 0.1mol/l hydrochloric acid dropwise under stirring at 25deg.C for titration, continuously recording pH value until pH becomes 4.05, and recording total volume consumed by hydrochloric acid as H p1 =22.09ml;
S12, weighing m u1 Placing 50.00g of leveling liquid to be tested in a standard beaker with 250ml, and preparing 150ml of leveling liquid diluent to be tested by deionized water under the constant temperature condition of stirring and 25 ℃; the pH detector is placed in the diluent of the leveling liquid to be detected, and 0.1mol/l hydrochloric acid is slowly added dropwise for titration under the constant temperature condition of stirring and 25 ℃ untilWhen the pH became 4.04, the total volume consumed by hydrochloric acid was recorded as H u1 =13.24ml;
S13, the concentration of alkaline substances in the leveling liquid to be measured is calculated as mass fraction C 1 The concentration of alkaline substances in the leveling liquid to be measured is calculated by the following formula:
s2, the concentration of acidic substances in the leveling liquid to be measured
S21, weighing m p2 Placing 5.10g of flattening stock solution in a 250ml standard beaker, adding 10g of glycerol reagent under the constant temperature condition of 55 ℃, preparing 150ml of flattening stock solution diluent by using deionized water, and keeping the constant temperature and stirring for 50min; the pH detector is placed in the flattening stock solution, 0.6mol/l potassium hydroxide solution is slowly added dropwise under the constant temperature condition of stirring and 55 ℃ for titration until the pH value becomes 11.05, and the total volume consumed by potassium hydroxide is recorded as H p2 =10.95ml;
S22, weighing m u2 Placing 49.95g of flattening liquid to be tested in a 250ml standard beaker, adding 10g of glycerol reagent under the constant temperature condition of 55 ℃, preparing 150ml of flattening liquid diluent to be tested by deionized water, and keeping the constant temperature and stirring for 50min; the pH detector is placed in the diluent of the leveling liquid to be detected, 0.6mol/l potassium hydroxide solution is slowly added dropwise for titration under the constant temperature condition of stirring and 55 ℃, and when the pH value becomes 11.04, the total volume consumed by the potassium hydroxide is recorded as H u2 =6.28ml;
S23, the concentration of acidic substances in the leveling liquid to be measured is calculated as mass fraction C 2 The concentration of acidic substances in the leveling liquid to be measured is calculated by the following formula:
s3, the concentration of the leveling liquid to be measured is calculated by mass fraction C TPL Representing, calculating the level to be measured usingConcentration of whole liquid, wherein the concentration influence coefficient a=0.55;
C TPL =[A·C 1 +(1-A)·C 2 ]·100%=5.93%
in the concentration detection process of the leveling liquid to be detected, the leveling liquid to be detected samples liquid from field use, and the concentration level of the leveling liquid in actual circulation can be truly reflected according to the concentration of 5.93% detected by the method in consideration of continuous leveling liquid use loss in production and errors in the addition process.
In combination with examples 1-4, the method for detecting the concentration of the cold rolling circulating leveling liquid fully considers the property of the cold rolling leveling liquid, and utilizes the acidity and alkalinity of chemical substances added in the leveling liquid to obtain the accurate concentration of the leveling liquid by carrying out acid-base titration treatment on the original leveling liquid and the cold rolling circulating leveling liquid used in the cold rolling production process; the method has the advantages of simple operation process, rapid detection result, wide practical prospect and high detection precision.
In view of the foregoing, the embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, and the scope of the claims of the present invention should be covered.

Claims (7)

1. A method for detecting the concentration of cold rolling circulation flattening liquid is characterized in that the consumption of acid and alkali in the flattening stock solution diluent and the flattening liquid diluent to be detected are respectively measured by acid-alkali titration to obtain the concentration of acidic substances and the concentration of alkaline substances in the flattening liquid to be detected, thereby obtaining the concentration of the flattening liquid to be detected,
the detection method comprises the following steps:
s1, preparing a flattening stock solution diluent and a flattening stock solution diluent to be tested respectively, then titrating the flattening stock solution diluent and the flattening stock solution diluent to be tested respectively by using hydrochloric acid until the pH value becomes 4+/-0.05, measuring the consumption of the hydrochloric acid in the flattening stock solution diluent and the flattening stock solution diluent to be tested, and calculating to obtain the concentration of alkaline substances in the flattening stock solution to be tested;
s2, respectively preparing a diluent of the leveling stock solution and a diluent of the leveling solution to be measured, then respectively titrating the diluent of the leveling stock solution and the diluent of the leveling solution to be measured by using a potassium hydroxide solution until the pH value becomes 11+/-0.05, measuring the consumption of potassium hydroxide in the diluent of the leveling stock solution and the diluent of the leveling solution to be measured, and calculating the concentration of acidic substances in the leveling solution to be measured;
s3, obtaining the concentration of the leveling liquid to be measured through the concentration of the alkaline substance and the concentration of the acidic substance in the leveling liquid to be measured,
the step S1 includes the steps of:
s11, weighing m p1 Placing 1-5 g of flattening stock solution into a standard beaker, and preparing 150m l of flattening stock solution diluent by deionized water; titration with hydrochloric acid until pH became 4.+ -. 0.05 was carried out, and the total volume consumed by hydrochloric acid was recorded as H p1
S12, weighing m u1 Placing 20-50 g of leveling liquid to be tested in a standard beaker, and preparing 150m l of leveling liquid diluent to be tested by deionized water; titration with hydrochloric acid until pH became 4.+ -. 0.05 was carried out, and the total volume consumed by hydrochloric acid was recorded as H u1
S13, the concentration of alkaline substances in the leveling liquid to be measured is calculated as mass fraction C 1 The concentration of alkaline substances in the leveling liquid to be measured is calculated by the following formula:
wherein C is 1 : concentration of alkaline substances in the leveling liquid to be measured,%;
H p1 : in the step S11, when the pH value is changed to 4+/-0.05 by titration with hydrochloric acid, the total volume of hydrochloric acid consumed by the stock solution diluent is leveled, and ml is leveled;
H u1 : in the step S12, when the pH value is changed to 4+/-0.05, the total volume of hydrochloric acid consumed by the diluent of the leveling liquid to be tested is ml;
m p1 : in the step S11, the mass of the weighed leveling stock solution, g;
m u1 : in step S12, the mass, g,
the step S2 includes the steps of:
s21, weighing m p2 Placing 1-5 g of flattening stock solution into a standard beaker, adding 5-20 g of glycerol reagent, preparing 150ml of flattening stock solution diluent by deionized water, and stirring for at least 20min; titration with potassium hydroxide solution until pH became 11.+ -. 0.05, the total volume consumed by potassium hydroxide was recorded as H p2
S22, weighing m u2 Placing 20-50 g of to-be-measured leveling liquid into a standard beaker, adding 5-10 g of glycerol reagent, preparing 150ml of to-be-measured leveling liquid diluent by deionized water, and stirring for at least 20min; titration with potassium hydroxide solution until pH became 11.+ -. 0.05, the total volume consumed by potassium hydroxide was recorded as H u2
S23, the concentration of acidic substances in the leveling liquid to be measured is calculated as mass fraction C 2 The concentration of acidic substances in the leveling liquid to be measured is calculated by the following formula:
wherein C is 2 : concentration of acidic substances in the leveling liquid to be measured,%;
H p2 : in the step S21, when the pH value is changed to 11+/-0.05, the total volume of potassium hydroxide consumed by the stock solution diluent is leveled, and ml is obtained;
H u2 : in the step S22, when the pH value is changed to 11+/-0.05, the total volume of the consumed potassium hydroxide in the diluent of the leveling liquid to be tested is ml;
m p2 : in the step S21, the mass of the weighed leveling stock solution, g;
m u2 : in step S22, the mass, g,
in the step S3, the to-be-measured levelingThe concentration of the liquid is expressed as mass fraction C TPL The concentration of the leveling liquid to be measured is calculated using the formula:
C TPL =[A·C 1 +(1-A)·C 2 ]·100%
wherein C is TPL : concentration of the leveling liquid to be measured,%;
a: concentration influence coefficient is a dimensionless value;
C 1 : concentration of alkaline substances in the leveling liquid to be measured,%;
C 2 : concentration of acidic substances in the leveling liquid to be measured,%.
2. The method for detecting the concentration of a cold rolling circulation leveling liquid according to claim 1, wherein in the step S11 and the step S12, the concentration of the hydrochloric acid is 0.005 to 0.1mol/l.
3. The method for detecting the concentration of a cold rolling circulation leveling liquid according to claim 1, wherein,
in the step S11, the flattening stock solution diluent is configured and titrated under the constant temperature condition of 20-25 ℃;
in the step S12, the diluent of the leveling liquid to be tested is configured and titrated under the constant temperature condition of 20-25 ℃.
4. The method for detecting the concentration of a cold rolling circulation leveling liquid according to claim 1, wherein in the step S21 and the step S22, the concentration of the potassium hydroxide solution is 0.02 to 0.6mol/l.
5. The method for detecting the concentration of a cold rolling circulation leveling liquid according to claim 1, wherein,
step S21, preparing and titrating the flattening stock solution diluent under the constant temperature condition of 30-55 ℃;
in the step S22, the diluent of the leveling liquid to be tested is configured and titrated under the constant temperature condition of 30-55 ℃.
6. The method for detecting the concentration of a cold rolling circulation leveling liquid according to claim 1, wherein in the step S5, the concentration influence coefficient a is 0.5 to 1.
7. The method for detecting the concentration of a cold rolling circulation leveling liquid according to claim 6, wherein the concentration influence coefficient A is 0.5 to 0.6.
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