CN109324025B - Method for monitoring water treatment agent content in circulating water system - Google Patents
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Abstract
The invention relates to a method for monitoring the content of a water treatment agent in a circulating water system. The method comprises the following steps: mixing and dissolving the dendritic macromolecules and the water treatment agent according to the mass ratio of 1:200 to prepare a fluorescence-labeled compound water treatment agent, and adding the compound water treatment agent into a circulating water system; selecting a wavelength of 200-600nm according to the fluorescence characteristic of a chromophore with a dendritic macromolecular structure, respectively measuring the fluorescence tracers in the compound water treatment agent by using a fluorescence spectrophotometer, and drawing a standard curve graph of fluorescence intensity and concentration under different concentrations in circulating water; and obtaining the concentration of the water treatment agent according to a standard curve corresponding to the fluorescence intensity, and timely supplementing the water treatment agent into the circulating water system when the water treatment agent is lower than the minimum effective concentration value. Has the advantages that: the tracer has the characteristics of high detection accuracy and stable performance.
Description
Technical Field
The invention relates to a method for monitoring the content of a water treatment agent in a circulating water system.
Background
In order to respond to the strategy of sustainable development, circulating water with the purpose of saving water is widely applied to the industrial field. In order to solve the problems of scaling, corrosion and fungus breeding on the surface of circulating water equipment, a certain amount of scale inhibitor, corrosion inhibitor and bactericide is usually added to achieve the aim. In order to obtain a good water treatment effect, it is critical to stabilize the concentration of the chemical within an effective range, in addition to selecting a high-efficiency chemical. At present, domestic circulating water systems generally adopt manual timing uniform dosing, effective values of medicament concentration in water are obtained through analysis, and the opening degree of a metering pump is adjusted according to the effective values. However, the volume of the system is too large, which may cause the data analysis to be delayed, the medicine to be wasted, and the system equipment to be damaged.
In order to better control the content of a water treatment agent of a circulating water system, save cost and prolong the service life of equipment, people monitor the agent in the water treatment system by a fluorescent tracing technology, and achieve the purpose of controlling a water treatment agent by monitoring the concentration of the fluorescent tracing agent, so that the water treatment agent is reasonably and efficiently utilized, and the stable operation of the circulating water system is ensured. Patent CN101726475A describes a semiconductor quantum dot fluorescent tracer, which is composed of nanocrystals composed of semiconductor materials and having fluorescent properties. The tracer and the water treatment agent are mixed and then added into an industrial water system, and the adding amount of the water treatment agent is controlled by continuously monitoring the concentration of the fluorescent tracer in the water system; patent CN106370632A describes a fluorescent tracer of sodium sulfanilate, which is prepared by physically blending sodium sulfanilate and a water treatment medicament according to a certain proportion, and measuring the fluorescence intensity of the compounded water treatment medicament to obtain the concentration of the water treatment medicament; patent CN107652256A describes an aqueous fluorescent tracer that is water soluble, low cost, chemically and biologically stable.
Although the reports on fluorescent tracers are increasing at present, most of the fluorescent tracers are benzene ring substances containing conjugated pi bonds, and the fluorescent tracers are complex in synthesis steps, difficult in subsequent treatment and single in type. Therefore, the development of fluorescent tracers with novel structures other than benzene ring structures is a trend of the development of circulating water systems. Therefore, it is necessary to provide an effective solution to the above problems.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for monitoring the content of a water treatment agent in a circulating water system. The monitoring method has high detection accuracy and stable performance.
The technical scheme for solving the technical problems is as follows:
a method for monitoring the content of water treatment agent in a circulating water system comprises the following steps:
(1) mixing and dissolving the dendritic macromolecules and the water treatment agent according to the mass ratio of 1:200, wherein the water treatment agent scale inhibitor comprises the following components in percentage by mass: corrosion inhibitor: the bactericide is mixed according to the ratio of 1:1:1 to prepare a fluorescence-labeled compound water treatment agent, and the fluorescence-labeled compound water treatment agent is added into a circulating water system.
(2) Selecting a wavelength of 200-600nm according to the fluorescence characteristic of the chromophore with the dendritic macromolecular structure, respectively measuring the fluorescent tracer in the compound water treatment agent by using a fluorescence spectrophotometer, and drawing a standard curve graph of fluorescence intensity and concentration under different concentrations in circulating water.
(3) And obtaining the concentration of the water treatment agent according to a standard curve corresponding to the fluorescence intensity, and timely supplementing the water treatment agent into the circulating water system when the water treatment agent is lower than the minimum effective concentration value.
Preferably, the dendrimer in step (1) comprises: one or more of 0.5G, 1.5G or 2.5G dendrimer products taking ethylenediamine as a core and 0.5G, 1.5G or 2.5G dendrimer products taking diethylenetriamine as a core.
Preferably, the water treatment agent in step (1) is: scale inhibitor polyepoxysuccinic acid, water soluble benzotriazole as corrosion inhibitor, or dodecyl dimethyl benzyl ammonium chloride as bactericide.
Preferably, the mass ratio of the dendritic macromolecule to the water treatment agent in the step (1) is 1: 200.
Preferably, the concentration of the fluorescent-labeled compound water treatment agent added into the circulating water system in the step (1) is as follows: 500 mg/L.
Preferably, the step (2) is to determine the fluorescence intensity of the tracer at different concentrations, wherein the concentration of the tracer is: 0.1mg/L, 0.5mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 7.0mg/L, 9.0 mg/L.
Has the advantages that: the tracer has the advantages of high detection accuracy and stable performance. The tracer and the water treatment agent are mixed for use and added into a circulating water system, the concentration of the fluorescent tracer in the circulating water system is monitored, the content of the water treatment agent is tracked, the water treatment agent is conveniently supplemented, and the concentration of the agent is ensured within an effective action range so as to ensure the scale inhibition, corrosion inhibition and sterilization effects of the circulating water system.
This kind of tracer can simply, the accurate fluorescence intensity of surveying through fluorescence spectrum analyzer, utilizes the peculiar fluorescence characteristic of dendrimer to carry out the medicament spike, and this tracer has the advantage that detection accuracy is high, the stable performance.
Drawings
In the drawings:
FIG. 1 is a standard curve of different generations of dendrimers with ethylenediamine as the core tracer of the present invention;
FIG. 2 is a standard curve of different generation numbers of dendrimers with the tracer diethylenetriamine as a core;
FIG. 3 is a standard curve of the concentration of 2.5G ethylenediamine cored dendrimer and 1.5G diethylenetriamine cored dendrimer of the present invention with water treatment agent concentration;
FIG. 4 is a standard curve of a dendrimer with a core of 2.5G ethylenediamine and a core of 1.5G diethylenetriamine in different proportions of the tracer of the present invention;
FIG. 5 is a standard curve of the concentration of 2.5G ethylenediamine cored dendrimer and 1.5G diethylenetriamine cored dendrimer of the tracer in different proportions with the concentration of water treatment agent;
in the figure: a: 2.5G dendrimer with ethylenediamine as core; b: 1.5G dendritic macromolecule with diethylenetriamine as core; r: fitting a curve linear correlation coefficient; 0.5G: a first step product of synthesis; 1.5G: the third step of synthesis; 2.5G: and (4) synthesizing a product in the fifth step.
Detailed Description
The application relates to a method for monitoring the content of a water treatment agent in a circulating water system, which comprises the following steps:
(1) mixing and dissolving the dendritic macromolecules and a water treatment agent according to a mass ratio of 1:200, wherein the water treatment agent is a scale inhibitor: corrosion inhibitor: mixing the bactericides according to the ratio of 1:1:1 to prepare a fluorescence-labeled compound water treatment agent, and adding the compound water treatment agent into a circulating water system;
(2) respectively measuring the fluorescent tracer in the compound water treatment agent by using a fluorescence spectrophotometer under the wavelength of 200-600nm, drawing the fluorescence intensity and concentration standard curve chart under different concentrations in circulating water;
(3) and obtaining the concentration of the water treatment agent according to a standard curve corresponding to the fluorescence intensity, and timely supplementing the water treatment agent into the circulating water system when the water treatment agent is lower than the minimum effective concentration value.
As an example of the present application, the dendrimer in step (1) includes: one of 0.5G, 1.5G or 2.5G dendrimer products with ethylenediamine as a core. Respectively preparing 0.5G of dendritic macromolecule taking ethylenediamine as core, 1.5G of dendritic macromolecule taking ethylenediamine as core and 2.5G of dendritic macromolecule taking ethylenediamine as core, wherein the standard concentrations of the dendritic macromolecules are 0.1mg/L, 0.5mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 7.0mg/L and 9.0mg/L, and adding a solvent to the solution at the lambda ofem/λexThe fluorescence intensity was measured at 425/370 wavelength and a standard curve was plotted (as shown in FIG. 1). According to the linear coefficient of the standard curve drawn by the product, the accuracy of the 2.5G ethylenediamine dendrimer product is higher.
Specifically, the synthesis steps of the dendritic macromolecules with different generations and ethylenediamine as the core are as follows:
putting 51.6G of methyl acrylate into a four-neck flask, dropwise adding a mixed solution of 6G of ethylenediamine and 20G of methanol in an ice-water bath, ensuring that the temperature is lower than 15 ℃, keeping the temperature at 25 ℃ for 24 hours after dropwise adding, and removing excessive raw materials and solvents by reduced pressure distillation to obtain a 0.5G product;
putting 18G of ethylenediamine and 50G of methanol into a four-neck flask, dropwise adding a mixed solution of 20.2G of 0.5G product and 20G of methanol in an ice-water bath, keeping the temperature at 25 ℃ for reaction for 24 hours after dropwise adding, and carrying out reduced pressure distillation to obtain 1.0G product;
putting 51.6G of methyl acrylate and 40G of methanol into a four-neck flask, dropwise adding a mixed solution of 25.8G of 1.0G product and 60G of methanol in an ice-water bath, reacting at the temperature of 25 ℃ for 24 hours, and distilling under reduced pressure to obtain a 1.5G product;
putting 36G of ethylenediamine and 70G of methanol into a four-neck flask, dropwise adding a mixed solution of 49.8G of 1.5G product and 50G of methanol in an ice water bath, keeping the temperature at 25 ℃ for reacting for 36 hours after dropwise adding, and carrying out reduced pressure distillation to obtain a 2.0G product;
putting 41.28G of methyl acrylate and 40G of methanol into a four-neck flask, dropwise adding a mixed solution of 22.4G of 2.0G product and 60G of methanol in an ice-water bath, reacting at the temperature of 25 ℃ for 36 hours, and distilling under reduced pressure to obtain 2.5G product.
As an example of the present application, the dendrimer in step (1) includes: one of 0.5G, 1.5G or 2.5G dendritic macromolecule products taking diethylenetriamine as a core. Respectively preparing 0.5G of dendritic macromolecule taking diethylenetriamine as a core, 1.5G of dendritic macromolecule taking diethylenetriamine as a core and 2.5G of dendritic macromolecule taking diethylenetriamine as a core, wherein the standard concentrations of the dendritic macromolecules are 0.1mg/L, 0.5mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 7.0mg/L and 9.0mg/L, and adding a solution of the solution into the solution at the lambda-positionem/λexThe fluorescence intensity was measured at 475/420 wavelength and a standard curve was plotted (as shown in FIG. 2). According to the linear coefficient of the standard curve drawn by the product, the accuracy of the 1.5G diethylenetriamine dendritic macromolecule product is higher.
Specifically, the synthesis steps of the dendritic macromolecules with different generations and taking diethylenetriamine as a core are as follows:
putting 68.8G of methyl acrylate into a four-neck flask, dropwise adding a mixed solution of 10.3G of diethylenetriamine and 40G of methanol in an ice-water bath, keeping the temperature below 15 ℃, keeping the temperature at 25 ℃ for 24 hours after dropwise adding, and removing excessive raw materials and solvents by reduced pressure distillation to obtain 0.5G of product;
putting 41.2G of diethylenetriamine and 120G of methanol into a four-neck flask, dropwise adding a mixed solution of 26.65G of 0.5G product and 20G of methanol in an ice-water bath, keeping the temperature at 25 ℃ for reaction for 24 hours after dropwise adding, and carrying out reduced pressure distillation to obtain 1.0G product;
putting 34.4G of methyl acrylate and 70G of methanol into a four-neck flask, dropwise adding a mixed solution of 17.76G of 1.0G product and 80G of methanol in an ice-water bath, carrying out heat preservation reaction at 25 ℃ for 36 hours, and carrying out reduced pressure distillation to obtain 1.5G product;
putting 51.5G of diethylenetriamine and 100G of methanol into a four-neck flask, dropwise adding a mixed solution of 87.4G of 1.5G product and 100G of methanol in an ice water bath, keeping the temperature at 25 ℃ for reaction for 36 hours after the dropwise adding is finished, and carrying out reduced pressure distillation to obtain a 2.0G product;
34.4G of methyl acrylate and 50G of methanol are put into a four-neck flask, a mixed solution of 49.16G of 2.0G product and 100G of methanol is dropwise added in an ice-water bath, the mixture is subjected to heat preservation reaction at 25 ℃ for 36 hours, and the mixture is subjected to reduced pressure distillation to obtain 2.5G product.
Table 1 shows the thermogravimetric analysis data results of different nuclei and different generations of products.
TABLE 1 thermogravimetric analysis data of different nuclei and different algebraic products
The data in table 1 are thermogravimetric analysis data of different nuclei and different generations of products, and the weight loss temperature and the weight loss ratio reflect the stability and the applicable temperature of the products. The data show that the weight loss temperature of the 2.5G product of the dendritic macromolecule taking the ethylenediamine as the core can reach 240 ℃ at most, and the weight loss ratio is 20.14% at least; the weight loss temperature of the 1.5G product of the dendrimer taking diethylenetriamine as the core is 255 ℃, and the weight loss ratio is 17.87 percent at the lowest, so that the 2.5G stability of the product taking ethylenediamine as the core is the best, and the 1.5G stability of the product taking diethylenetriamine as the core is the best.
The present invention will be described in detail with reference to the following examples, but the scope of the present invention is not limited to the following embodiments.
Example 1
2.5G dendritic macromolecule product with ethylenediamine as core, and scale inhibitor (polyepoxysuccinic acid): corrosion inhibitor (water soluble benzotriazole): the bactericide (dodecyl dimethyl benzyl ammonium chloride) is mixed with a water treatment medicament in a ratio of 1:1:1, and the content of the bactericide is monitored by a fluorescence method, and the method comprises the following steps:
(1) taking 0.1G of dendritic macromolecule taking 2.5G of ethylenediamine as core and 20G of mixed water treatment agent, mixing and dissolving in a beaker according to the proportion of 1:200, uniformly stirring by magnetic force, transferring into a 100ml volumetric flask, and preparing into 500mg/L of fluorescence labeling compound water treatment agent;
(2) then, a solution of 0.1mg/L, 0.5mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 7.0mg/L, 9.0mg/L of dendrimer with 2.5G of ethylenediamine as a core was prepared at lambdaem/λexThe fluorescence intensity was measured at 425/370 wavelength and a standard curve was plotted. Along with the continuous consumption of the water treatment agent, the concentration of the dendritic macromolecule taking the 2.5G ethylenediamine as the core in the solution is gradually increased, the fluorescence intensity is gradually enhanced, and the concentration of the corresponding water treatment agent is obtained by combining the measured fluorescence intensity with the corresponding standard curve.
Example 2
1.5G dendritic macromolecule product with diethylenetriamine as core, and scale inhibitor (polyepoxysuccinic acid): corrosion inhibitor (water soluble benzotriazole): the bactericide (dodecyl dimethyl benzyl ammonium chloride) is mixed with a water treatment medicament in a ratio of 1:1:1, and the content of the bactericide is monitored by a fluorescence method, and the method comprises the following steps:
(1) taking 0.1G of dendritic macromolecule taking 1.5G of diethylenetriamine as a core and 20G of mixed water treatment agent, mixing and dissolving in a beaker according to the proportion of 1:200, uniformly stirring by magnetic force, transferring into a 100ml volumetric flask, and preparing into 500mg/L of fluorescence labeling compound water treatment agent;
(2) then preparing solution with 1.5G diethylenetriamine as core and dendrimer concentration of 0.1mg/L, 0.5mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 7.0mg/L and 9.0mg/L at lambdaem/λexThe fluorescence intensity was measured at 475/420 wavelength and a standard curve was plotted. Along with the continuous consumption of the water treatment agent, the concentration of the dendritic macromolecule taking 1.5G diethylenetriamine as a core in the solution is gradually increased, the fluorescence intensity is gradually enhanced, and the concentration of the corresponding water treatment agent is obtained by combining the measured fluorescence intensity with the corresponding standard curve.
Example 3
Taking 2.5G of dendritic macromolecule taking ethylenediamine as core and 1.5G of dendritic macromolecule taking diethylenetriamine as core, and mixing the raw materials according to the weight ratio of 1:1, 1:1.2, 1:1.4 and 1: 1.6, 1:1.8 and 1:2 to obtain the mixed dendritic macromolecular fluorescent tracer, wherein the ratio of the scale inhibitor (polyepoxysuccinic acid): corrosion inhibitor (water soluble benzotriazole): the bactericide (dodecyl dimethyl benzyl ammonium chloride) is mixed with a water treatment medicament in a ratio of 1:1:1, and the content of the bactericide is monitored by a fluorescence method, and the method comprises the following steps:
(1) respectively taking 0.1g of a dendritic macromolecular mixed product and 20g of a mixed water treatment agent in different proportions, mixing and dissolving in a beaker according to the proportion of 1:200, uniformly stirring by magnetic force, transferring into a 100ml volumetric flask, and preparing into 500mg/L of a fluorescence-labeled compound water treatment agent;
(2) then, solutions having concentrations of 0.1mg/L, 0.5mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 7.0mg/L, and 9.0mg/L were prepared, and fluorescence intensities were measured at specific wavelengths to draw a calibration curve. And (3) along with the continuous consumption of the water treatment agent, the concentration of the dendritic macromolecules in the solution is gradually increased, the fluorescence intensity is gradually enhanced, and the concentration of the corresponding water treatment agent is obtained by combining the measured fluorescence intensity with a corresponding standard curve. According to the linear coefficient of the standard curve drawn by the product, 2.5G of ethylenediamine dendrimer can be known: the accuracy of the product is higher when the 1.5G dendritic macromolecule taking diethylenetriamine as the core is 1: 1.2.
FIG. 3 is a standard curve diagram showing the relationship between the concentration of 2.5G ethylenediamine-cored dendrimer and the concentration of 1.5G diethylenetriamine-cored dendrimer and the concentration of the water treatment agent, and with reference to FIGS. 1 and 2, the concentration of the water treatment agent can be obtained according to the measured fluorescence intensity of the tracer, so as to determine whether the agent needs to be added.
FIG. 4 examines the relationship between the fluorescence intensity and the tracer concentration under different proportions of 2.5G ethylene diamine as core dendrimer and 1.5G diethylene triamine as core dendrimer, so as to obtain a mixed fluorescent tracer with higher accuracy.
Fig. 5 examines a standard curve chart of concentration and concentration of the water treatment agent under different proportions of 2.5G of ethylenediamine as core dendrimer and 1.5G of diethylenetriamine as core dendrimer, and in combination with fig. 4, the concentration of the water treatment agent can be obtained according to the measured fluorescence intensity of the tracer, so as to judge whether water treatment agent needs to be added.
The method for monitoring the content of the water treatment agent in the circulating water system is realized by the following steps: the method comprises the steps of mixing the fluorescent tracer and a water treatment medicament, enabling the using dosage to be 0.1-10 mg/L, adding the mixture into a circulating water system, monitoring the fluorescence intensity of the fluorescent tracer in the system to obtain the concentration of the tracer, and rapidly and accurately obtaining the content value of the water treatment medicament by monitoring the concentration value of the tracer due to the fact that the concentrations of the tracer and the water treatment medicament have correlation.
And (3) along with the consumption of the water treatment agent, the concentration of the dendritic tracer agent is gradually increased, the fluorescence intensity of the dendritic tracer agent is gradually enhanced, the concentration of the water treatment agent is obtained according to a standard curve corresponding to the fluorescence intensity, and when the water treatment agent is lower than the minimum effective concentration value, the water treatment agent is timely supplemented into the circulating water system.
The dendrimer used in the invention is a novel compound with a three-dimensional structure, the compound has a large number of cavities inside and a large number of active groups outside, and the synthesis method is simple, good in water solubility and stable in property.
Claims (4)
1. A method for monitoring the content of a water treatment agent in a circulating water system is characterized by comprising the following steps:
(1) mixing and dissolving the dendritic macromolecules and a water treatment agent according to a mass ratio of 1:200, wherein the water treatment agent is a scale inhibitor: corrosion inhibitor: mixing the bactericides according to the ratio of 1:1:1 to prepare a fluorescence-labeled compound water treatment agent, and adding the fluorescence-labeled compound water treatment agent into a circulating water system;
the dendrimer includes: one or more of 0.5G, 1.5G or 2.5G dendritic macromolecule products taking ethylenediamine as a core;
the water treatment agent is: scale inhibitor polyepoxysuccinic acid, water soluble benzotriazole as corrosion inhibitor and dodecyl dimethyl benzyl ammonium chloride as bactericide;
(2) respectively measuring the fluorescent tracer in the compound water treatment agent by using a fluorescence spectrophotometer under the wavelength of 200-600nm, drawing the fluorescence intensity and concentration standard curve chart under different concentrations in circulating water;
(3) and obtaining the concentration of the water treatment agent according to a standard curve corresponding to the fluorescence intensity, and timely supplementing the water treatment agent into the circulating water system when the water treatment agent is lower than the minimum effective concentration value.
2. The method of monitoring according to claim 1, wherein the dendrimer in step (1) is a combination of a 2.5G dendrimer product having an ethylenediamine core and a 1.5G dendrimer product having a diethylenetriamine core, and the weight ratio of the 2.5G dendrimer product having an ethylenediamine core to the 1.5G dendrimer product having a diethylenetriamine core is 1: 1.2.
3. the method of claim 1, wherein the fluorescently labeled compound water treatment agent added to the circulating water system in step (1) has a concentration of: 500 mg/L.
4. The method of claim 1, wherein the step (2) comprises measuring the fluorescence intensity of the tracer at different concentrations of the tracer, wherein the concentration of the tracer is: 0.1mg/L, 0.5mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 7.0mg/L, 9.0 mg/L.
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