CN114487225A - Method for measuring sulfur and chlorine content in fly ash - Google Patents
Method for measuring sulfur and chlorine content in fly ash Download PDFInfo
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- CN114487225A CN114487225A CN202210066697.7A CN202210066697A CN114487225A CN 114487225 A CN114487225 A CN 114487225A CN 202210066697 A CN202210066697 A CN 202210066697A CN 114487225 A CN114487225 A CN 114487225A
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- G—PHYSICS
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- G—PHYSICS
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Abstract
The invention discloses a method for measuring the content of sulfur and chlorine in fly ash, belonging to the field of chemical component analysis and test. Specifically, the measurement method comprises: mixing fly ash with manganese oxide and anhydrous sodium carbonate to obtain a first mixture, then spreading a second mixture obtained by mixing copper oxide and anhydrous sodium carbonate on the first mixture, heating to 750-850 ℃ in an oxygen-containing atmosphere, preserving heat for 30-150 min, performing water immersion extraction on the obtained intermediate, and measuring the sulfur content and the chlorine content in the extracting solution. Wherein the weight ratio of fly ash, manganese oxide and anhydrous sodium carbonate in the first mixture is 1: (0.05-1): (0.5 to 3); the weight ratio of the copper oxide to the anhydrous sodium carbonate in the second mixture is (1-5): 1. the determination method is simple and easy to operate, can be used for simultaneously and rapidly determining the chlorine and sulfur content in the fly ash, and has the advantages of stable result, good accuracy and high accuracy.
Description
Technical Field
The invention relates to the field of chemical component analysis and test, in particular to a method for measuring sulfur and chlorine content in fly ash.
Background
The production amount of the waste incineration fly ash is increased year by year, and the fly ash contains a large amount of chlorine and sulfide. The existence of chloride increases the treatment difficulty of the waste incineration fly ash, the chloride can corrode cement reinforcing steel bars in the cement solidification treatment of the fly ash, the cement aging is accelerated, and sulfide enhances the fly ash solidification effect. During the heat treatment of the fly ash, the chlorides increase the volatilization of the heavy metals, and the opposite sulfides can increase the solidification rate of the heavy metals. The detection of the chlorine and sulfur content of the fly ash is a necessary task before the fly ash is treated and disposed.
The analysis of chlorine and sulfur content in the waste incineration fly ash has no complete set of standards, and generally, the method for measuring the chlorine in the coal comprises a high-temperature combustion hydrolysis-potentiometric titration method and an Eschka mixture sample melting-potassium bisulfate titration method; the method for measuring the sulfur in the coal comprises the following steps: the Eschka method, the coulometric titration method, the high-temperature combustion neutralization method; the method for measuring the chlorine in the cement comprises the following steps: ammonium thiocyanate volumetric method of nitric acid decomposition, silver sulfate automatic titration method of nitric acid decomposition and ion chromatography; the method for measuring the sulfur in the cement comprises the following steps: iodometry. However, these methods can only measure the content of one element singly.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for measuring the sulfur and chlorine content in fly ash, which can simultaneously and rapidly measure the sulfur content and the chlorine content in the fly ash.
In order to solve the problems, the invention discloses a method for measuring the content of sulfur and chlorine in fly ash, which comprises the following steps:
(1) mixing fly ash with manganese oxide and anhydrous sodium carbonate to obtain a first mixture;
(2) spreading the first mixture into a container and spreading a predetermined amount of a second mixture over the first mixture;
(3) heating the second mixture to 750-850 ℃ in an oxygen-containing atmosphere, and preserving heat for 30-150 min to obtain an intermediate;
(3) soaking and extracting the intermediate in water to obtain an extracting solution;
(4) measuring the sulfur content and the chlorine content in the extracting solution;
wherein in the first mixture, the weight ratio of fly ash, manganese oxide and anhydrous sodium carbonate is 1: (0.05-1): (0.5 to 3);
the second mixture is a mixture of copper oxide and anhydrous sodium carbonate, and the weight ratio of the second mixture is (1-5): 1.
specifically, sulfur in the fly ash reacts with anhydrous sodium carbonate and manganese oxide to form soluble substances such as sodium sulfate and magnesium sulfate. A small amount of sulfur in the form of metal sulfide is decomposed with manganese oxide in a high temperature process to produce O2React to form SO2、SO3And then is coveredThe anhydrous sodium carbonate absorbs the reaction product to form soluble substances such as sodium sulfate, magnesium sulfate and the like. In addition, a small amount of overflowing sulfur dioxide and sulfur trioxide can be absorbed by copper oxide.
Most of the chlorine in the fly ash is present in the form of soluble substances such as sodium chloride, potassium chloride, manganese chloride, arsenic chloride, chromium chloride, etc., and the chlorine in these forms is not changed during the treatment. A small amount of chloride ion type hydrotalcite and lead chloride which exist in an insoluble form react with manganese oxide, anhydrous sodium carbonate and copper oxide at high temperature to form soluble substances such as magnesium chloride, sodium chloride and copper chloride.
In addition, alumina and iron oxide carried by the fly ash react with metal chloride at high temperature to form hydrogen chloride, and the hydrogen chloride can be absorbed by anhydrous sodium carbonate and manganese oxide, so that the hydrogen chloride is added into the intermediate obtained by roasting in the form of soluble magnesium chloride and sodium chloride.
As an improvement of the technical scheme, in the first mixture, the weight ratio of fly ash, manganese oxide and anhydrous sodium carbonate is 1 (0.05-0.2): (0.5-2). By controlling the dosage proportion, the measured rate (measured amount/actual total amount) of sulfur and chlorine in the fly ash can reach more than 95%.
As an improvement of the above technical solution, the weight ratio of the first mixture to the second mixture is 1: (1-2).
As an improvement of the above technical solution, in the second mixture, the weight ratio of copper oxide to anhydrous sodium carbonate is (1.5-2.5): 1.
as an improvement of the technical scheme, in the step (2), the temperature of the mixture is firstly increased to 780-800 ℃, the temperature increasing time is 15-28 min, and then the temperature is maintained at 780-800 ℃ for 100-120 min.
In the step (2), the temperature raising and maintaining step is performed in a tube furnace.
As an improvement of the technical scheme, the step (3) comprises the following steps:
(3.1) cooling the intermediate to 20-30 ℃;
(3.2) dispersing the intermediate in water to obtain a dispersion liquid;
(3.3) heating the dispersion to 150-250 ℃ and maintaining for 10-30 min; heating and then carrying out ultrasonic treatment for 5-10 min;
and (3.4) cooling the dispersion liquid obtained in the step (3.3) to 20-30 ℃, standing and precipitating, and taking supernatant liquid to obtain an extracting solution.
As an improvement of the above technical scheme, in the step (4), Cl in the extracting solution is measured by adopting ion chromatography-Content and SO4 2-And (4) content.
Further, in the measurement of Cl in the extract-Content and SO4 2-After the content, the content of Cl and S in the fly ash is converted by the following two formulas:
wherein, wCl、wSRespectively the chlorine content and the sulfur content in the fly ash (%),
for Cl in the extract-The content (mg/L) of (A),
is SO in the extract4 2-Content (mg/L); and m is the mass of the fly ash sample.
As an improvement of the technical scheme, the fly ash is waste incineration fly ash.
The implementation of the invention has the following beneficial effects:
the present invention mixes fly ash with manganese oxide and anhydrous sodium carbonate, then calcines them at specific temp., then extracts them by water immersion, and converts all Cl and S existed in various forms in fly ash into Cl by the above-mentioned technological process-And SO4 2-And then the measurement is performed. The method can simultaneously and rapidly detectThe content of chlorine and sulfur in the fly ash is measured, and the result is stable, accurate and high in accuracy.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below.
Example 1
Weighing 1.0000 +/-0.0002 g of dried fly ash sample, 1g of manganese oxide and 0.5g of anhydrous sodium carbonate, putting the dried fly ash sample, the manganese oxide and the anhydrous sodium carbonate into a 23mL corundum ark, fully mixing, uniformly mixing 4.5g of copper oxide and 1g of anhydrous sodium carbonate, and then flatly paving the mixture on the surface of the mixture in the ark. Placing the ark in a tube furnace, plugging the ark into a furnace plug, heating to 840 ℃ for 35min for 20min, naturally cooling to room temperature after baking, transferring the substances in the corundum ark into a 250mL beaker, washing the ark three times by deionized hot water, and transferring the substances into the beaker together. Adding deionized water into a beaker containing a sample to a scale mark of 75mL, heating to 150 ℃ on an electric hot plate, maintaining for 10min, then carrying out ultrasonic treatment for 5min, cooling to room temperature, standing for precipitation, then carrying out inclined method to filter supernatant, and repeating the steps to the residual residue for primary leaching (heating and ultrasonic treatment). Filtering the solution residue after the second leaching, cleaning the inner wall of the beaker for 3 times, diluting the filtrate to 200mL with deionized water, and measuring Cl in the solution by ion chromatography-、SO4 2-。
Example 2
Weighing 1.0000 +/-0.0002 g of dried fly ash sample, 0.5g of manganese oxide and 1.5g of anhydrous sodium carbonate, putting the weighed materials into a 23mL corundum ark, fully mixing, uniformly mixing 3g of copper oxide and 1g of anhydrous sodium carbonate, and then flatly paving the mixture on the surface of the mixture in the ark. Placing the ark in a tube furnace, plugging the ark into a furnace plug, heating to 840 ℃ for 35min for 20min, naturally cooling to room temperature after baking, transferring the substances in the corundum ark into a 250mL beaker, washing the ark three times by deionized hot water, and transferring the substances into the beaker together. Adding deionized water into beaker containing sample to 75mL scale mark, heating to 150 deg.C on electric heating plate, maintaining for 10min, performing ultrasonic treatment for 5min, cooling to room temperature, standing for precipitation, filtering supernatant by tilting method, and collecting residueThe above steps are repeated for one leaching (heating + sonication). Filtering the solution residue after the second leaching, cleaning the inner wall of the beaker for 3 times, diluting the filtrate to 200mL with deionized water, and measuring Cl in the solution by ion chromatography-、SO4 2-。
Example 3
Weighing 1.0000 +/-0.0002 g of dried fly ash sample, 0.2g of manganese oxide and 1.8g of anhydrous sodium carbonate, putting the weighed materials into a 23mL corundum ark, fully mixing, uniformly mixing 3g of copper oxide and 1g of anhydrous sodium carbonate, and then flatly paving the mixture on the surface of the mixture in the ark. Placing the ark in a tube furnace, plugging the ark into a furnace plug, heating to 840 ℃ for 35min for 20min, naturally cooling to room temperature after baking, transferring the substances in the corundum ark into a 250mL beaker, washing the ark three times by deionized hot water, and transferring the substances into the beaker together. Adding deionized water into a beaker containing a sample to a scale mark of 75mL, heating to 150 ℃ on an electric hot plate, maintaining for 10min, then carrying out ultrasonic treatment for 5min, cooling to room temperature, standing for precipitation, then carrying out inclined method to filter supernatant, and repeating the steps to the residual residue for primary leaching (heating and ultrasonic treatment). Filtering the solution residue after the second leaching, cleaning the inner wall of the beaker for 2-3 times, diluting the filtrate to 200mL with deionized water, and measuring Cl in the solution by ion chromatography-、SO4 2-。
Example 4
Weighing 1.0000 +/-0.0002 g of dried fly ash sample, 0.2g of manganese oxide and 1.8g of anhydrous sodium carbonate, putting the weighed materials into a 23mL corundum ark, fully mixing, uniformly mixing 2.5g of copper oxide and 1g of anhydrous sodium carbonate, and then flatly paving the mixture on the surface of the mixture in the ark. Placing the ark in a tube furnace, plugging the ark into a furnace plug, heating to 840 ℃ for 35min for 20min, naturally cooling to room temperature after baking, transferring the substances in the corundum ark into a 250mL beaker, washing the ark three times by deionized hot water, and transferring the substances into the beaker together. Adding deionized water into beaker containing sample to 75mL scale mark, heating to 150 deg.C on electric heating plate, maintaining for 10min, performing ultrasonic treatment for 5min, cooling to room temperature, standing for precipitation, filtering supernatant by tilting method, and collecting the residueThe slag is extracted once again by repeating the above steps (heating + ultrasound). Filtering the solution residue after the second leaching, cleaning the inner wall of the beaker for 2-3 times, diluting the filtrate to 200mL with deionized water, and measuring Cl in the solution by ion chromatography-、SO4 2-。
Example 5
Weighing 1.0000 +/-0.0002 g of dried fly ash sample, 0.2g of manganese oxide and 1.8g of anhydrous sodium carbonate, putting the weighed materials into a 23mL corundum ark, fully mixing, uniformly mixing 2.5g of copper oxide and 1g of anhydrous sodium carbonate, and then flatly paving the mixture on the surface of the mixture in the ark. Placing the ark in a tube furnace, plugging the ark into a furnace plug, heating to 800 ℃ for 110min for 30min, naturally cooling to room temperature after baking, transferring the substances in the corundum ark into a 250mL beaker, washing the ark three times by deionized hot water, and transferring the substances into the beaker together. Adding deionized water into a beaker containing a sample to a scale mark of 75mL, heating to 150 ℃ on an electric hot plate, maintaining for 10min, then carrying out ultrasonic treatment for 5min, cooling to room temperature, standing for precipitation, then carrying out inclined method to filter supernatant, and repeating the steps to the residual residue for primary leaching (heating and ultrasonic treatment). Filtering the solution residue after the second leaching, cleaning the inner wall of the beaker for 2-3 times, diluting the filtrate to 200mL with deionized water, and measuring Cl in the solution by ion chromatography-、SO4 2-。
Comparative example
The method of GB/T214-2007 is adopted to measure the total sulfur in the fly ash. Reference is made to the method of Kaixing Zhao, Yuyan Hu, Yuyi Tian, De zhen Chen, Yuxing Feng, Chlorine removal from MSWI flash by thermal treatment, Effects of ion/aluminum additives [ J ]. Journal of Environmental Sciences,2020,88(C) for determination of total chlorine in fly ash. And used as an evaluation criterion.
Comparative example 1
The difference between this comparative example 1 and example 4 is that a 1g fly ash sample was first mixed well with 2g magnesium oxide and 1g anhydrous sodium carbonate, and then a mixture of 2g magnesium oxide and 1g anhydrous sodium carbonate was laid flat.
Comparative example 2
This comparative example is different from example 4 in that only 2g of anhydrous sodium carbonate was mixed with fly ash in the first mixing step, and the rest was the same as example 4.
Comparative example 3
This comparative example differs from example 4 in that only 3g of anhydrous sodium carbonate was tiled in the second tiling step. The rest is the same as in example 4.
Comparative example 4
This comparative example is different from example 4 in that fly ash, 0.2g of manganese oxide, 2.8g of anhydrous sodium carbonate, and 2g of copper oxide were directly mixed, and the rest was the same as example 4.
Comparative example 5
This comparative example is different from example 4 in that the temperature is increased to 900 ℃ for 30min and maintained for 35min, and the rest is the same as example 4.
Comparative example 6
This comparative example differs from example 4 in that the temperature was raised to 700 ℃ for 20min and maintained for 35min, the remainder being the same as example 4.
The examples 1 to 5 and the comparative examples 1 to 6 were repeated 3 times each, and the average value was used to calculate the measurement rate, which was calculated by the following formula:
wherein eta isiIs the measured rate of the i-th group,
is the average of the chlorine content or the sulfur content of group i, wisThe average value of the chlorine content or the sulfur content measured in the control example was used.
Specific test data are shown in the following table:
as can be seen from examples 1 to 5, the measuring method of the present invention has Cl and S measuring rates of not less than 97%. As can be seen from comparison between example 4 and comparative examples 2 to 6, when the combination of the agents of the present invention was changed or the parameters such as the feeding method and the temperature system were changed, the measurement rate decreased and the effect of the present invention was hardly achieved. In addition, as can be seen from the comparison between the comparative example 1 and the example 4, the traditional Eschka reagent has difficulty in accurately measuring the sulfur and chlorine contents in the fly ash.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (9)
1. A method for measuring the content of sulfur and chlorine in fly ash is characterized by comprising the following steps:
(1) mixing fly ash with manganese oxide and anhydrous sodium carbonate to obtain a first mixture;
(2) spreading the first mixture into a container and spreading a predetermined amount of a second mixture over the first mixture;
(3) heating the second mixture to 750-850 ℃ in an oxygen-containing atmosphere, and preserving heat for 30-150 min to obtain an intermediate;
(3) soaking and extracting the intermediate in water to obtain an extracting solution;
(4) measuring the sulfur content and the chlorine content in the extracting solution;
wherein in the first mixture, the weight ratio of fly ash, manganese oxide and anhydrous sodium carbonate is 1: (0.05-1): (0.5 to 3);
the second mixture is a mixture of copper oxide and anhydrous sodium carbonate, and the weight ratio of the second mixture is (1-5): 1.
2. the method for measuring the content of sulfur and chlorine in the fly ash according to claim 1, wherein the weight ratio of the fly ash, the manganese oxide and the anhydrous sodium carbonate in the first mixture is 1 (0.05-0.2): (0.5-2).
3. The method for measuring the sulfur and chlorine content in fly ash according to claim 1, wherein the weight ratio of the first mixture to the second mixture is 1: (1-2).
4. The method for measuring the content of sulfur and chlorine in fly ash according to claim 1, wherein the weight ratio of the copper oxide to the anhydrous sodium carbonate in the second mixture is (1.5-2.5): 1.
5. the method for measuring the content of sulfur and chlorine in fly ash according to claim 1, wherein in the step (2), the temperature of the mixture is raised to 780-800 ℃ for 15-28 min, and then the temperature is maintained at 780-800 ℃ for 100-120 min.
6. The method according to claim 1, wherein the temperature raising and maintaining step is carried out in a tube furnace in step (2).
7. The method for measuring the content of sulfur and chlorine in fly ash according to claim 1, wherein the step (3) comprises:
(3.1) cooling the intermediate to 20-30 ℃;
(3.2) dispersing the intermediate in water to obtain a dispersion liquid;
(3.3) heating the dispersion to 150-250 ℃ and maintaining for 10-30 min; heating and then carrying out ultrasonic treatment for 5-10 min;
and (3.4) cooling the dispersion liquid obtained in the step (3.3) to 20-30 ℃, standing and precipitating, and taking supernatant liquid to obtain an extracting solution.
8. The method for measuring the content of sulfur and chlorine in fly ash according to claim 1, wherein in the step (4), the Cl in the extracting solution is measured by ion chromatography-Content and SO4 2-And (4) content.
9. The method for measuring the sulfur and chlorine content in fly ash according to claim 1, wherein the fly ash is waste incineration fly ash.
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