CN113670764A - Hydrothermal accelerated experiment method for batch safety detection of stability of steel slag granules - Google Patents
Hydrothermal accelerated experiment method for batch safety detection of stability of steel slag granules Download PDFInfo
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- 239000002893 slag Substances 0.000 title claims abstract description 193
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 185
- 239000010959 steel Substances 0.000 title claims abstract description 185
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000002474 experimental method Methods 0.000 title claims abstract description 23
- 238000001514 detection method Methods 0.000 title claims abstract description 22
- 239000008187 granular material Substances 0.000 title claims abstract description 10
- 238000010298 pulverizing process Methods 0.000 claims abstract description 57
- 238000006243 chemical reaction Methods 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002245 particle Substances 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000005303 weighing Methods 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 238000007873 sieving Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims description 19
- 238000010998 test method Methods 0.000 claims description 13
- 229920006395 saturated elastomer Polymers 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 31
- 238000005070 sampling Methods 0.000 abstract description 7
- 230000035484 reaction time Effects 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000002791 soaking Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 17
- 239000000395 magnesium oxide Substances 0.000 description 9
- 235000012245 magnesium oxide Nutrition 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000000292 calcium oxide Substances 0.000 description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 5
- 239000000428 dust Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 238000007667 floating Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 4
- 238000006703 hydration reaction Methods 0.000 description 4
- 238000004445 quantitative analysis Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000007654 immersion Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 230000001133 acceleration Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
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- 230000029087 digestion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 239000009346 wu-tou Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The invention discloses a hydrothermal accelerated experiment method for batch safety detection of stability of steel slag granules, which comprises the following steps: firstly, selecting a plurality of steel slag samples to be detected in batches at one time, and washing and drying the steel slag samples; then respectively adding the mixture into a reaction kettle, adding water for soaking, and placing the mixture into an oven for hydrothermal reaction; taking out and drying each fully cooled steel slag sample, weighing m mass of product after hydrothermal reaction of the steel slag in each reaction kettle0Sieving the steel slag with a 1.18mm sieve, and weighing the mass m of the steel slag obtained below the sieve1And calculating the pulverization rate of each steel slag particle material according to the proportion of the two. The invention firstly proposes that the reaction kettle is adopted to replace the traditional large autoclave (with the volume of 8500mL) for testing the steel slag pulverization rate, so that simultaneous determination of various samples at one time can be realized, the working strength is greatly reduced, and the processing period is shortened; the oven can be opened for sampling test at any different reaction time; the aim of measuring the stability of the steel slag aggregate in batches and safely is achieved at a relatively low temperature.
Description
Technical Field
The invention belongs to the technical field of material testing methods, and particularly relates to a batch safety detection method for stability of steel slag.
Background
The essence of the stability problem of the steel slag is that the stability of the steel slag is directly determined by the content of expansion components (free calcium oxide, periclase, simple substance iron and RO phase) contained in the steel slag and the digestion/hydration degree. When the steel slag is applied to building materials, the use environment is mostly alkaline environment, and the volume stability problem caused by the simple substance iron is generally concerned a little (the simple substance iron is generally not oxidized in the alkaline environment); the RO phase causes the problem of volume stability mainly because the RO phase contains MgO (the content of the periclase which can be incorporated) or FeO (the MgO and the FeO are not oxidized under the alkaline environment), so that most of the standards generally concern the content of free calcium oxide and periclase when evaluating the volume stability of the steel slag by adopting an expansion component, but the free calcium oxide and the periclase undergo high-temperature melting in the smelting process and are in a dead burning state, the activity is low, the hydration reaction is slow, and therefore, the expansion damage formed in the slow reaction process of a hydration product has a long latency period. At present, various methods for testing the stability of the steel slag are also mainly started from two aspects: on one hand, the content of f-CaO and periclase is detected by a chemical method generally, but the determination of the content of the f-CaO is a local weight in China, and the determination of the content of the periclase does not give sufficient attention; on the other hand, the volume stability of the steel slag is used for judging, and different testing methods are provided according to different requirements of different application fields on the size of steel slag particles in the aspect, wherein the testing methods comprise the stability, the pulverization rate, the mortar rod linear expansion rate and the like of the steel slag under the water immersion or boiling or autoclaving conditions. The latter, namely, the volume stability of steel slag, is generally used for judging the steel slag granules used as aggregates.
The domestic and foreign determination of the volume stability of the steel slag stipulates different detection methods according to the particle size of the steel slag aggregate and the application field. The method is combined with the standards of GB/T32546-. For the steel slag coarse aggregate, if the steel slag coarse aggregate is applied to road base materials, asphalt pavement aggregates and engineering backfilling (the maximum grain diameter can reach 53mm), the stability of the steel slag aggregate is generally evaluated by a water-soaking expansion rate experimental method; if the steel slag particles are applied to mortar or concrete, the stability of the steel slag aggregate is generally evaluated by the autoclaving pulverization rate or the autoclaving expansion rate; for the application of the ground steel slag powder in cement and concrete, the stability of the steel slag powder product is generally detected by boiling or pressure steaming stability according to a cement stability detection method. The national standard common method for testing the steel slag granules comprises the autoclaving pulverization rate, the autoclaving expansion rate and the water immersion expansion rate, and for the water immersion expansion rate, because the difficulty coefficient of test piece manufacture is larger, the test period is longer, and most of the test pieces are adopted in the field of highway engineering, the stability can not be considered in the process of rapid evaluation. And to the test of present autoclaving pulverization rate or autoclaving expansion rate, though compare greatly shortening with the test method of soaking expansion rate on the test cycle, still there is the predicament that a plurality of samples of sample can't be tested simultaneously fast when many, and adopt when the autoclave because the autoclave is bulky sealed degree of difficulty coefficient is big, generally need hold special type operating certificate and the big personnel of strength carry out the operation of symmetrical tightening sealing screw, the complicated messenger test cycle of operating process that relates to is long, the security is poor and the process is loaded down with trivial details.
The corresponding measurement principle of the traditional autoclaving and pulverization rate is as follows: the expansion components in the steel slag are subjected to accelerated hydration reaction at a higher temperature by utilizing the autoclaving environment, so that part of the steel slag is disintegrated, the particle size is reduced, and the stability of the steel slag can be judged according to the disintegration degree of the steel slag. The specific determination process is that the steel slag is treated by saturated steam at 215.7 ℃ for 3h, and is autoclaved under the corresponding pressure of 2.0MPa (the appearance of a typical autoclave is shown in figure 1), so that free calcium oxide and free magnesium oxide contained in the steel slag are digested and expanded and pulverized into small particles, and the stability of the steel slag is judged by the pulverization rate. The equipment for determining the autoclaving and pulverization rate specified in the national standard is an autoclave, and the following technical problems exist when the autoclave is adopted: 1) due to high temperature and high pressure, only a person holding a special operation certificate can use the device in consideration of safety during laboratory application; 2) the sample cannot be added randomly in the midway, and the rapid test cannot be carried out when a large number of samples exist; 3) the autoclave can be opened by the cooperation of a plurality of people during use, and the operation is complex, time-consuming and labor-consuming. With the application and popularization of the steel slag granules, a technology for testing the stability of the steel slag in a large scale needs to be further explored urgently.
Disclosure of Invention
The invention mainly aims to provide a hydrothermal accelerated experiment method for batch safety detection of stability of steel slag granules, aiming at the problems and the defects in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
a hydrothermal accelerated experiment method for batch safety detection of stability of steel slag granules comprises the following steps:
1) selecting a plurality of steel slag samples to be detected in batches at one time, wherein each sample is steel slag with the grain size of 1.18-2.36mm, and preparing a plurality of parallel steel slag samples; washing with water, and drying at 100-110 ℃ to a saturated dry state; 2) respectively adding the steel slag samples obtained by the treatment in the step 1) into a reaction kettle, adding water to soak the steel slag samples, and sealing; then placing the reaction kettle (the appearance of the typical reaction kettle is shown in figure 2) in an oven with the temperature of 179.5-180.5 ℃ for hydrothermal reaction for 23.5-24.5 h;
3) taking out the reaction kettle, cooling, taking out the fully cooled steel slag sample from the reaction kettle, shaking the steel slag adhered to the wall of the reaction kettle into a disc in a shaking-off mode, and washing the residual steel slag with water; the sample loss during sampling is avoided, then the sample is dried and weighed, and the mass of the steel slag sample after the hydrothermal reaction is recorded as m0To the nearest 0.1 g;
4) drying the mixture obtained in the step 3)Sieving the obtained steel slag sample by a 1.18mm sieve until the throughput per minute is less than 0.1 percent of the total amount of the sample, weighing the steel slag under the sieve and recording the mass as m1；
5) Calculating the steel slag pulverization rate f according to a formula:
preferably, the types of the steel slag samples to be detected are more than 8; the parallel samples of each steel slag sample are more than 3; the number of the reaction kettles placed in the oven is more than 24.
In the scheme, after a proper amount of steel slag aggregate is selected by the steel slag through a quartering method, the steel slag aggregate is crushed to the particle size of 1.18-2.36mm to obtain the steel slag aggregate.
In the scheme, the volume of the reaction kettle is 100-500 mL; preferably 100mL, 150mL, 200mL, 300mL, 400mL, 500mL, or the like.
Preferably, the addition amount of the steel slag in the reaction kettle is 120-300 g.
Preferably, the water is added in the step 2) in an amount which is 0.95-1.05 cm higher than the steel slag and is completely wetted.
In the scheme, the cooling step in the step 3) can adopt a flowing water rapid cooling or natural cooling mode; preferably, the flowing water rapid cooling mode is adopted, and when the flowing water rapid cooling mode is adopted, the cooling time is 20min at the ambient temperature of 20 ℃.
Preferably, the sieving step comprises: and (3) adopting a simple hand-operated screening mode or placing the screen on a screen shaker to shake for 9.5-10.5 min and then manually operating the screen until the throughput per minute is less than 0.1% of the total amount of the sample.
In the scheme, the water can be distilled water or pure tap water.
In the scheme, the steel slag sample to be detected is one or more of hot stuffy steel slag, roller steel slag, hot splashing steel slag and the like in different batches.
Preferably, the number of the reaction kettles placed in the oven is 24 or more, so that synchronous detection of steel slag samples of different types or sources can be realized, and the detection efficiency can be remarkably improved.
The invention realizes the purpose of rapidly and safely measuring the stability of the steel slag aggregate at relatively low temperature under the condition of adjusting the proper experimental reaction temperature and reaction time.
Compared with the prior art, the invention has the beneficial effects that:
1) the quantitative analysis method for detecting the steel slag pulverization rate can realize batch, safe, efficient and rapid determination, and is particularly suitable for the condition of many steel slag samples; therefore, the total time consumption of the detection process is greatly reduced, the test result is accurate, the quantitative analysis result of the hydrothermal pulverization rate of the steel slag is accurate to 0.01 percent, the numerical value is reduced according to GB/T8170, and the test result meets the precision requirement and the actual requirement.
2) The quantitative analysis method for the steel slag pulverization rate is simple in detection process, safe and non-toxic, the detection process mainly relates to setting of the temperature of an oven (such as 180 ℃), tightening and placing of a reaction kettle (without cooperation of multiple persons and small tightening force and convenient operation), and taking out and quick cooling after reaction time is reached, compared with the steps of sealing and fastening (requiring cooperation of multiple persons and large tightening force, which cannot be completed by common female laboratory staff alone) and slow pressure release cooling and the like when a traditional autoclave is used as a reaction container, the test method has the advantages of being simpler in process, safer, more convenient and the like.
3) In the quantitative analysis method for the steel slag pulverization rate, multiple samples can be placed at one time in the detection process, and the samples can be added at any time in the middle, so that the batch rapid detection of different types of steel slag samples can be realized.
Drawings
FIG. 1 is a structural diagram of a ZYF-2 type autoclave adopted in a traditional autoclave pulverization rate test method.
FIG. 2 is a structural diagram of a reaction kettle used in the hydrothermal acceleration experimental method of the present invention.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the content of the present invention, but the present invention is not limited to the following examples.
Example 1
An accelerated experiment method for batch safety detection of stability of steel slag aggregate comprises the following specific steps:
1) weighing two samples of the steel slag with the grain size of 1.18mm-2.36mm and the steel slag with the steel drum with the steel grain size meeting the requirement, wherein the weighing value of each sample is 120 g; 3 slag samples prepared in parallel for each sample were used for testing; before testing, washing the weighed steel slag particles with water, washing away floating dust and impurities on the surface of the steel slag, filtering to remove water, and putting the steel slag particles to (or drying properly) a saturated surface dry state;
2) respectively putting the obtained slag samples into 6 reaction kettle containers of 150mL, adding 65g of water into each kettle to ensure that the water completely wets the steel slag and is higher than the steel slag by about 1.0cm, putting the reaction kettle filled with the soaked slag samples into a drying oven of 180 ℃ for hydrothermal reaction for 24 hours, and then turning off a power supply; taking out the reaction kettle and rapidly cooling by flowing water;
3) the steel slag after being fully cooled is carefully taken out of the reaction kettle and placed in a disc, the steel slag adhered to the wall of the reaction kettle is shaken off into the disc, the residue is properly washed by distilled water, and sample loss during sampling is avoided in an experiment; then dried and weighed, and recorded as m0To the nearest 0.1 g;
4) then sieving the dried steel slag by a 1.18mm sieve, firstly placing the sieve on a sieve shaker to shake for 20min, and then manually shaking the sieve until the throughput per minute is less than 0.1 percent of the total amount of the sample; steel slag mass m under balance weighing screen1；
5) According to the formula I, the hydrothermal pulverization rates of 3 slag samples of the Wu-Tou steel hot disintegration steel slag are respectively 12.78%, 12.72% and 12.81%, the average value of 3 parallel samples is 12.77%, and the standard deviation of the parallel samples is 4.6%;
the hydrothermal pulverization rates of 3 slag samples of the Wu-Steel roller steel slag are respectively 4.12%, 4.17% and 4.18% according to the formula I, the average value of 3 parallel samples is 4.15%, and the standard deviation of the parallel samples is 3.2%.
Aiming at the wu-steel hot smoldering steel slag in the embodiment, the average value of the autoclaving pulverization rate is 12.28% by further adopting the traditional autoclaving pulverization rate method (saturated steam treatment at 215.7 ℃ for 3h, and the corresponding pressure is 2.0 MPa). The result shows that the hydrothermal pulverization rate value obtained by the hydrothermal pulverization rate method is very close to the autoclaving pulverization rate value, the absolute value difference is 0.49%, and the relative error is 3.99%; can accurately represent the stability of the steel slag.
Aiming at the steel slag of the Wu steel roller in the embodiment, the average value of the autoclaving pulverization rate is tested to be 4.25% by adopting the traditional autoclaving pulverization rate method. The result shows that the hydrothermal pulverization rate value obtained by the test of the hydrothermal pulverization rate method is very close to the autoclaving pulverization rate value, the absolute value difference is 0.20 percent, and the relative error is 2.35 percent; can accurately represent the stability of the steel slag.
Example 2
An accelerated experiment method for batch safety detection of stability of steel slag aggregate comprises the following specific steps:
1) weighing 120g of steel slag subjected to hot splashing of steel with the Wu steel and the particle size of 1.18mm-2.36mm, wherein the particle size of the steel slag meets the requirement, and parallelly preparing 3 slag samples for testing; before testing, washing the weighed hot splashing steel slag particles with water, washing away floating dust and impurities on the surface of the steel slag, filtering to remove water, and putting the steel slag to (or drying properly) a saturated surface dry state;
2) respectively putting the obtained slag samples into 3 reaction kettle containers of 150mL, adding 65g of water, putting the reaction kettle filled with the immersed slag samples into a drying oven of 180 ℃ for hydrothermal reaction for 24 hours, and then turning off a power supply; then directly taking out the reaction kettle and naturally cooling to room temperature;
3) the steel slag after being fully cooled is carefully taken out of the reaction kettle and placed in a disc, the steel slag adhered to the wall of the reaction kettle is shaken off into the disc, the residue is properly washed by distilled water, and sample loss during sampling is avoided in an experiment; then dried and weighed, and recorded as m0To the nearest 0.1 g;
4) then sieving the dried steel slag through a 1.18mm sieve, and shaking the sieve by hand until the throughput per minute is less than 0.1 percent of the total amount of the sample; steel slag mass m under balance weighing screen1；
5) According to the formula I, the hydrothermal pulverization rates of 3 slag samples of the Wu-Steel hot splashing steel slag are 27.89%, 27.81% and 27.86%, the average value of the 3 parallel slag samples is 27.85%, and the standard deviation of the parallel samples is 4.0%.
Aiming at the steel slag subjected to hot splashing of the Wu Steel, the average value of the autoclaving and pulverization rate of the steel slag is 27.82 percent by adopting a traditional autoclaving and pulverization rate test method. The result shows that the hydrothermal pulverization rate value obtained by the test of the hydrothermal pulverization rate method is very close to the value of the autoclaving pulverization rate, the absolute value difference is 0.03%, and the relative error is 0.11%; can accurately represent the stability of the steel slag.
Example 3
An accelerated experiment method for batch safety detection of stability of steel slag aggregate comprises the following specific steps:
1) weighing 300g of steel slag with the grain size of 1.18mm-2.36mm and the steel slag with the grain size meeting the requirement, and parallelly preparing 3 slag samples for testing; before testing, washing the weighed roller steel slag particles with water, washing away floating dust and impurities on the surface of the steel slag, filtering to remove water, and putting the steel slag particles to (or drying properly) a saturated surface dry state;
2) respectively putting the obtained slag samples into 3 reaction kettle containers with the volume of 500mL, adding 180g of water, putting the reaction kettle filled with the immersed slag samples into a drying oven with the temperature of 180 ℃ for hydrothermal reaction for 24 hours, and then turning off a power supply; then directly taking out the reaction kettle and naturally cooling to room temperature;
3) the steel slag after being fully cooled is carefully taken out of the reaction kettle and placed in a disc, the steel slag adhered to the wall of the reaction kettle is shaken off into the disc, the residue is properly washed by distilled water, and sample loss during sampling is avoided in an experiment; then dried and weighed, and recorded as m0To the nearest 0.1 g;
4) then sieving the dried steel slag through a 1.18mm sieve, and shaking the sieve by hand until the throughput per minute is less than 0.1 percent of the total amount of the sample; steel slag mass m under balance weighing screen1；
5) The hydrothermal pulverization rates of the 3 hot stuffy slag samples of the Wu steel are respectively 12.56%, 12.52% and 12.58% according to the formula I, the average value of the 3 parallel slag samples is 12.55%, and the standard deviation of the parallel samples is 4.0%. Aiming at the wu-steel hot smoldering steel slag in the embodiment, the autoclaving pulverization rate is further tested to be 12.28% by adopting the traditional autoclaving pulverization rate method. The result shows that the hydrothermal pulverization rate value obtained by the test of the hydrothermal pulverization rate method is very close to the autoclaving pulverization rate value, the absolute value difference is 0.27 percent, and the relative error is 2.20 percent; can accurately represent the stability of the steel slag.
Example 4
An accelerated experiment method for batch safety detection of stability of steel slag aggregate comprises the following specific steps:
1) selecting 8 steel slag samples (steel slag samples of steel slag hot splashing and steel slag of hot stuffiness) from different sources (different batches), respectively weighing 120g of steel slag samples with the particle size of 1.18-2.36mm, wherein the particle size of the steel slag samples meets the requirement, and parallelly preparing 3 steel slag samples for testing; before testing, washing the weighed steel slag particles with water, washing away floating dust and impurities on the surface of the steel slag, filtering to remove water, and putting the steel slag particles to (or drying properly) a saturated surface dry state;
2) respectively putting the 24 obtained slag samples into 24 reaction kettle containers with the volume of 150mL, adding 65g of water, putting the reaction kettle filled with the immersed slag samples into a drying oven with the temperature of 180 ℃ for hydrothermal reaction for 24 hours, and then turning off a power supply; taking out the reaction kettle and rapidly cooling by flowing water;
3) taking out the steel slag in the 24 fully cooled reaction kettles filled with the steel slag, placing the steel slag in a tray, shaking the steel slag adhered to the wall of the reaction kettle into the tray in a shaking-off mode, and properly washing the residue with distilled water to avoid sample loss during sampling in the experiment; then drying and weighing;
4) then sieving each steel slag sample by a 1.18mm sieve, wherein one part of the steel slag sample can be sieved by a sieve shaker, and the other part of the steel slag sample can be sieved by a hand, and the mass of the steel slag sieved by the sieve is weighed by using a balance after the steel slag sample is sieved to the specified requirement;
5) the hydrothermal pulverization rate of each steel slag sample calculated according to formula I is shown in Table 2.
Table 2 hydrothermal pulverization rate data of 8 samples (different kinds and batches) measured at once
The results in table 2 show that the hydrothermal pulverization rate of 8 steel slags can be obtained by one-time test by adopting the hydrothermal pulverization rate method, and the stability conditions of different batches of steel slags can be very conveniently and accurately distinguished.
Comparative example
In order to compare and analyze the rationality of the experimental temperatures (respectively corresponding to different experimental pressures) selected by the accelerated experimental method, 120 ℃, 150 ℃, 180 ℃, 200 ℃ and 215.7 ℃ are respectively selected, wherein 215.7 ℃ is the traditional autoclave experimental temperature and is used for carrying out corresponding comparison experiments. The method comprises the following specific steps:
1) selecting hot splashing steel slag samples of the same batch, weighing 120g of steel slag with the particle size of 1.18-2.36mm and the particle size meeting the requirement, and parallelly preparing 24 slag samples for testing; before testing, washing the weighed steel slag particles with water, washing away floating dust and impurities on the surface of the steel slag, filtering to remove water, and putting the steel slag particles to (or drying properly) a saturated surface dry state;
2) dividing 24 slag samples into 3 groups, respectively placing 8 150mL reaction kettle container samples filled with 120g of steel slag samples and 65g of water in 4 drying ovens, respectively setting the temperatures of the drying ovens to 120 ℃, 150 ℃, 180 ℃ and 200 ℃, respectively carrying out hydrothermal reaction for 3 hours and 24 hours, respectively taking out the samples from the drying ovens after the samples reach the specified time, carrying out subsequent experiments, and calculating the hydrothermal pulverization rates under different hydrothermal reaction conditions after the experiments are finished;
3) the other 3 samples are tested by adopting a traditional autoclave pulverization rate test method, and the obtained data are used for comparison;
4) the hydrothermal pulverization rate and the autoclaving pulverization rate of each steel slag sample at different reaction temperatures, which are respectively calculated according to the formula I, are shown in Table 3.
TABLE 3 hydrothermal pulverization Rate data for samples under different hydrothermal conditions
The results in table 3 show that the numerical difference of the hydrothermal pulverization rates at different experimental temperatures is very large, when the hydrothermal temperature of 120 ℃ or 150 ℃ and the reaction time of 3h and 24h are adopted, the data is far from the data obtained by the traditional autoclaving method, and the phenomenon of acceleration and slowing down appears along with the prolonging of the time under the condition of relatively low hydrothermal temperature; the difference between the pulverization rate obtained by 24h hydrothermal at 200 ℃ and the absolute value of the traditional autoclaving pulverization rate is 1.39%, so that the pulverization rate detection accuracy cannot be ensured; in addition, under such temperature conditions, the saturated steam will reach a high pressure condition of 1.57MPa or more, which further causes problems in the safety and operability of the reaction vessel.
The difference between the hydrothermal pulverization rate test method of the invention and the traditional autoclaving pulverization rate test method is shown in Table 4.
TABLE 4 comparison of two pulverization rates of steel slag granules (according to single experiment)
Injecting: although the autoclave pressure is reduced from 2MPa to 0.1MPa for 90min, the surface temperature of the autoclave is very high, the operation of screwing the cover with the heat-insulating gloves is inconvenient and easy to scald, and meanwhile, the autoclave is large in volume and cannot be cooled by running water, so that the surface temperature of the autoclave is continuously reduced to the operable temperature by adopting a natural cooling mode, and then sampling is carried out. Therefore, the actual pressure reduction and temperature reduction time generally needs about 4 hours.
As can be seen from Table 4, compared with the traditional autoclaving and pulverization method, the detection method of the invention can realize the rapid and accurate test of multiple types (different batches or steel slag types) at one time; the operation flow is obviously simplified, the operation difficulty is reduced, the workload is greatly reduced, the processing period is shortened, and the method is suitable for popularization and application.
The above embodiments are merely examples for clearly illustrating the present invention and do not limit the present invention. Other variants and modifications of the invention, which are obvious to those skilled in the art and can be made on the basis of the above description, are not necessary or exhaustive for all embodiments, and are therefore within the scope of the invention.
Claims (9)
1. A hydrothermal accelerated experiment method for batch safety detection of stability of steel slag granules is characterized by comprising the following steps:
1) selecting a plurality of steel slag samples to be detected in batches at one time, wherein each sample is steel slag with the grain size of 1.18-2.36mm, and preparing a plurality of parallel samples; washing with water, and drying to saturated dry state;
2) respectively adding the steel slag sample obtained by the treatment in the step 1) into each reaction kettle, adding water to soak the steel slag sample, and sealing; then placing the reaction kettle in an oven with the temperature of 179.5-180.5 ℃ for hydrothermal reaction for 23.5-24.5 h;
3) taking out the reaction kettle, cooling, taking out the steel slag sample after full cooling from the reaction kettle, drying and weighing, and recording the mass of the steel slag sample after hydrothermal reaction as m0To the nearest 0.1 g;
4) sieving the steel slag sample dried in the step 3) by a 1.18mm sieve until the throughput per minute is less than 0.1 percent of the total amount of the sample, and weighing the steel slag obtained under the sieve to obtain the mass m1；
5) Calculating the hydrothermal pulverization rate f of the steel slag according to a formula:
2. the hydrothermal accelerated experiment method as set forth in claim 1, wherein the types of the steel slag samples to be tested are more than 8; the parallel samples of each steel slag sample are more than 3; the number of the reaction kettles placed in the oven is more than 24.
3. The hydrothermal accelerated test method as defined in claim 1, wherein the steel slag is obtained by selecting a proper amount of steel slag aggregate through a quartering method and then crushing the steel slag aggregate to a particle size of 1.18-2.36 mm.
4. The hydrothermal accelerated test method as set forth in claim 1, wherein the volume of the reaction kettle is 100-500 mL.
5. The hydrothermal accelerated test method as set forth in claim 1, wherein the amount of the steel slag added in the reaction kettle is 120-300 g.
6. The hydrothermal accelerated test method according to claim 1, wherein the water is added in the step 2) in an amount of 0.95-1.05 cm higher than the fully wetted steel slag.
7. The hydrothermal accelerated test method as set forth in claim 1, wherein the cooling step in step 3) is performed by flowing water rapid cooling or natural cooling.
8. The hydrothermal accelerated test method according to claim 1, wherein the sieving step comprises: and (3) adopting a simple hand-operated screening mode or placing the screen on a screen shaker to shake for 9.5-10.5 min and then manually operating the screen until the throughput per minute is less than 0.1% of the total amount of the sample.
9. The hydrothermal accelerated experiment method as defined in claim 1, wherein the steel slag sample to be tested is one or more of hot stuffy steel slag, roller steel slag and hot splashing steel slag of different batches.
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