CN113060913B - Optimization method for carrying out harmless treatment on strongly alkaline red mud by utilizing easily-obtained industrial waste - Google Patents
Optimization method for carrying out harmless treatment on strongly alkaline red mud by utilizing easily-obtained industrial waste Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses an optimization method for performing harmless treatment on red mud which is industrial waste residue by utilizing easily obtained industrial waste. The method comprises the steps of mixing and stirring flue gas desulfurization residues and bittern with a red mud aqueous solution, and then pressing the mud to remove water to obtain the treated red mud. The method fully considers the current situation that the red mud contains alkaline substances which are quickly and slowly released, determines the proportion and the respective usage amount of alkaline neutralizing materials required for neutralizing the alkaline substances which are quickly and slowly released through a series of treatments, uses industrial waste flue gas desulfurization slag and bittern as the neutralizing materials, and utilizes the easily obtained and cheap industrial waste to carry out harmless treatment on the red mud which is also the industrial waste residue.
Description
Technical Field
The invention belongs to the field of red mud treatment, and particularly relates to an optimization method for carrying out harmless treatment on strongly alkaline red mud by utilizing easily-obtained industrial waste.
Background art:
the red mud produced during the production of alumina by the bayer process or the combined bayer-sintering process is strongly basic (pH typically greater than 11) and therefore corrosive. In order to safely dispose of the industrial waste residue, the alumina plant needs to spend a large amount of capital to build a red mud disposal site. Because the red mud is not suitable for plant growth, the naked red mud storage yard is easy to become a source ground which is harmful to human and animal health and raises dust. The alkalinity of the red mud is reduced, the corrosivity of the red mud can be eliminated, and conditions are created for soil conversion or resource utilization of the red mud. The alkalinity of red mud cannot be completely assessed by pH. Different red mud can have very different alkalities. In addition, red mud contains alkaline substances which are released quickly and slowly. The relative proportions of the two in red mud also vary depending on the type of red mud. The existing red mud treatment method does not fully consider the differences of the red mud. In order to improve the efficiency of red mud treatment, the alkalinity of the red mud needs to be characterized so as to determine the proportion of alkali neutralizing materials required for quickly neutralizing and slowly releasing alkali substances and the respective usage amount.
In order to reduce the treatment cost of the red mud, industrial waste which is easy to obtain and has strong neutralization effect on water-soluble alkaline substances of the red mud should be adopted as much as possible. However, industrial waste materials often contain impurities, and the content of the impurities varies greatly depending on the source. Therefore, there is a need to determine their neutralizing capacity for water-soluble bases before using these industrial wastes. At present, an effective method for measuring the capability of industrial waste for neutralizing water-soluble alkaline substances of red mud is lacked.
The invention content is as follows:
for the reasons, the invention aims to provide an optimization method for performing harmless treatment on red mud which is industrial waste residue by using easily available and cheap industrial waste.
The invention relates to an optimization method for performing harmless treatment on red mud which is also industrial waste residue by utilizing easily-obtained industrial waste, which is to mix and stir flue gas desulfurization slag and bittern with a red mud aqueous solution, and then squeeze the mud to remove water to obtain the treated red mud.
Preferably, the specific steps are as follows:
raw materials: red mud, flue gas desulfurization slag and bittern;
a. measuring the content of gypsum in the flue gas desulfurization slag, measuring the content of magnesium ions in bittern, and converting into magnesium chloride;
b. and (3) measuring the alkalinity of the red mud water extract:
adding 10 g of dried red mud into 50 ml of deionized water, oscillating on an oscillator for 1 hour, taking 25ml of extracting solution, continuously titrating the 25ml of extracting solution by using 0.05M HCl solution until the pH value is 7, and obtaining the alkalinity of the water extracting solution of the red mud by using the following formula according to the volume of the consumed HCl solution:
alkalinity (millimole/kg) of the red mud water extract is 2v × 0.05 × 100 v ═ 10 v; wherein v is the number of milliliters of HCl solution consumed by titrating the red mud water extract;
c. method for measuring total alkalinity of red mud
Taking 10 g of dried red mud, adding 20 ml of 0.05M hydrochloric acid solution to obtain red mud suspension, continuously titrating the red mud suspension by using 0.05M HCl solution until the pH value of the final point is 7, and calculating the total alkalinity of the red mud by using the following formula according to the volume of the consumed HCl solution:
total alkalinity (millimole/kg) — (v +20) × 0.05 × 100 ═ v +20) x5 of red mud
V in the above formula is the number of milliliters of HCl solution consumed by titration of the red mud suspension;
d. removal of OH in red mud by calcium sulfate - The capacity (millimole/kg) of 1000/86 × 1000 is 11627;
according to the designed dose-response experiment, continuously monitoring the pH of the reaction solution, wherein the detection time is 10, 25 and 50 hours after the test is started, if the pH is not close to 9 after 50 hours, measuring the pH once again every 25 hours until the pH is close to 9, and determining the addition amount of the pure gypsum required for reducing the pH of the red mud to be less than 9, namely the actual weight ratio of the calcium sulfate to the red mud;
e. removal of OH in red mud by magnesium chloride - Capacity (millimole/kg) of 1000/101.5X 1000 9852
Magnesium chloride/red mud ratio (alkalinity of red mud water extract/9852)
f. Carrying out comprehensive analysis and determining the weight ratio of magnesium chloride to calcium sulfate during red mud treatment to be
The actual calcium sulphate/red mud weight ratio: the ratio of magnesium chloride to red mud is equal to the weight ratio of magnesium chloride to calcium sulfate;
then determining the dosage of bittern and flue gas desulfurization slag when treating the red mud according to the content of gypsum in the flue gas desulfurization slag and the content of magnesium chloride in the bittern;
g. the method for measuring the water content of the red mud is characterized in that the dosage of bittern and flue gas desulfurization slag obtained by calculating the dried red mud is converted into the dosage of fresh red mud;
h. inputting the red mud into a reaction tank, and mixing the raw materials according to the weight ratio of the red mud: adding water according to the weight ratio of 1:2.5, adding bittern and flue gas desulfurization slag with the amount not less than the amount determined in the step g, stirring, inputting slurry into a filter press, and conveying the squeezed red mud to a storage yard. The squeezed water is recycled.
Preferably, the determination of the content of the gypsum in the flue gas desulfurization slag is directly performed by using an X-ray fluorescence spectrometer (XRF) and an X-ray diffractometer (XRD).
Preferably, the determination of the content of magnesium ions in the bittern is performed by using an inductively coupled plasma optical emission spectroscopy (ICP-OES) instrument or an atomic absorption spectrometer (ASS).
The method fully considers the current situation that the red mud contains alkaline substances which are quickly and slowly released, determines the proportion and the respective usage amount of alkaline neutralizing materials required for neutralizing the alkaline substances which are quickly and slowly released through a series of treatments, uses industrial waste flue gas desulfurization slag and bittern as the neutralizing materials, and utilizes the easily obtained and cheap industrial waste to carry out harmless treatment on the red mud which is also the industrial waste residue.
Description of the drawings:
FIG. 1 is a dose-response curve for sample 2;
FIG. 2 is a dose-response curve for sample 3;
FIG. 3 is a schematic view of a red mud treatment apparatus.
The specific implementation mode is as follows:
the following examples are further illustrative of the present invention and are not intended to be limiting thereof.
Example 1: determination of alkalinity of red mud
Three different red mud samples were selected: sample 1pH was 10.06; sample 2pH 11.27; sample 3 had a pH of 12.97.
1. The method for measuring the alkalinity of each red mud water extract comprises the following steps: approximately 10 g of dried red mud (accurate to 0.01 g) was placed in a 100 ml plastic bottle with a lid, 50 ml of deionized water was added, shaken on a shaker for 1 hour, 25ml of extract was taken, and 25ml of extract was titrated continuously with 0.05M standardized HCl solution on an autotitrator to the end point (pH 7). According to the volume of the consumed HCl solution, the alkalinity of the water extract of the red mud is calculated by the following formula:
alkalinity (millimole/kg) of extract of red mud water 2v x 0.05x 100 10v
In the above formula, v is the number of milliliters of HCl solution consumed for titrating the extract of red mud water.
2. The method for measuring the total alkalinity of the red mud comprises the following steps: about 10 g of dried red mud (accurate to 0.01 g) was taken, 20 ml of 0.05M solution of standardized hydrochloric acid (HCl) was added, and the red mud suspension was titrated continuously to the end point (pH 7) with 0.05M solution of standardized HCl on an autotitrator. According to the volume of the consumed HCl solution, the total alkalinity of the red mud is obtained by the following formula:
total alkalinity (millimole/kg) of red mud, (v +20) x 0.05x 100, (v +20) x5
In the above formula v is the number of ml of HCl solution consumed for titrating the red mud suspension.
3. The slow release alkalinity of the red mud is the difference between the total alkalinity of the red mud and the alkalinity of the red mud water extract, and is calculated by the following formula:
the alkalinity of red mud released slowly (millimole/kg) ═ total alkalinity of red mud-alkalinity of red mud water extract
The alkalinity of the red mud water extract and the total alkalinity of the red mud were obtained from the above three samples, and the results are shown in Table 1
TABLE 1
| Consumption of 0.05M HCl volume (ml) | Alkalinity (millimole/kg) | |
| Alkalinity of aqueous extract of sample 1 | 4.15 | 41.5 |
| Sample 1 Total alkalinity of Red mud | 65.9 | 429.5 |
| Sample 2 aqueous extract alkalinity | 11.5 | 115 |
| Sample 2 Total alkalinity of Red mud | 128.3 | 741.5 |
| Sample 3 aqueous extract alkalinity | 16.3 | 163 |
| Sample 3 Total alkalinity of Red mud | 439.7 | 2298.5 |
Example 2: determining the proportion of the treating agent to the red mud
1. Determining to remove OH in the red mud according to the total alkalinity of the red mud measured by the samples 2 and 3 - The desired theoretical calcium sulfate/red mud weight ratio. The dose-response experiment was designed accordingly and the pH of the reaction solution was monitored continuously for the 10 th, 25 th and 50 th hours after the start of the experiment. If the pH is not close to 9 after 50 hours, the measurement is performed again every 25 hours until the pH is close to 9. Determining the pure gypsum required for reducing the pH of the red mud to below 9, namely calcium sulfate dihydrate (CaSO) 4 ·2H 2 O) is added. The method comprises the following specific steps:
removing OH from red mud by calcium sulfate (i.e. calcium sulfate dihydrate, the same applies below) - Capacity (mmol/kg) of 1000/86 × 1000 11627
Therefore, the number of the first and second electrodes is increased,
the weight ratio of calcium sulfate/red mud of sample 2 was 741.5 (mmol/kg)/11627 (mmol/kg) 0.064
The weight ratio of calcium sulfate/red mud of sample 3 was 2298.5 (mmol/kg)/11627 (mmol/kg) was 0.198
Accordingly, the calcium sulfate additive amount interval of the sample 2 is set to be the ratio of calcium sulfate/red mud of 0 to 0.1; sample 3 the calcium sulfate additive dosage interval was between 0 and 0.4 calcium sulfate/red mud ratio.
In actual operation, a group (6 parts) of dried red mud (accurate to 0.01 g) with the weight of 50 g is weighed for each sample and put into a plastic bottle with the volume of 150 ml, and different amounts of pure calcium sulfate are respectively added. The calcium sulfate/red mud weight ratios for sample 2 were set at 0, 0.03, 0.05, 0.07, 0.09, and 1.00. The calcium sulfate/red mud weight ratios for sample 3 were set at 0, 0.01, 0.02, 0.05, 0.3, and 0.4. After adding calcium sulfate, respectively adding 100 ml of pure water into each bottle, tightly covering the bottle cap, oscillating on an oscillator for 10 hours, and then measuring the pH value of the solution; then continuing to oscillate the sample for 15 hours and then measuring the pH value of the solution again; the sample was then shaken for an additional 25 hours before the pH of the solution was again measured. At this point the pH was still not close to 9, so the shaking and pH measurements were continued every 25 hours. Sample 2 had a pH drop below 9 (fig. 1) after 50 hours of shaking, whereas sample 3 had a pH approaching 9 after 170 hours (fig. 2). From the dose-response curve it was determined that to reduce the pH of the red mud sample 2 below 9, the calcium sulfate/red mud ratio needed to reach 0.07. For the red mud sample 3 with higher alkalinity, the effect of reducing the alkalinity of the red mud is the best when the ratio of calcium sulfate to red mud reaches 0.4.
2. The alkalinity of the aqueous extracts of samples 2 and 3 is determined to rapidly eliminate free OH in the red mud - Magnesium chloride hexahydrate (MgCl) 2 ·6H 2 O) to determine the magnesium chloride/red mud weight ratio.
The method comprises the following specific steps:
removing OH in red mud by magnesium chloride (namely magnesium chloride hexahydrate) - Capacity (millimole/kg) of 1000/101.5X 1000 9852
Therefore, the number of the first and second electrodes is increased,
the ratio of magnesium chloride/red mud of sample 2 is 115 (mmol/kg)/9852 (mmol/kg) 0.012
Sample 3 had a magnesium chloride/red mud ratio of 163 (mmol/kg)/9852 (mmol/kg) of 0.017
3. Carrying out comprehensive analysis and determining the weight ratio of magnesium chloride to calcium sulfate when processing the red mud as follows:
sample 2 has 0.012/0.07 ═ 0.17 magnesium chloride/calcium sulfate (i.e., 1.7:10)
Sample 3 has 0.017/0.4 ═ 0.04 parts of magnesium chloride/calcium sulfate (i.e., 0.4:10)
Example 3: on-site treatment of fresh red mud in factory
1. During on-site construction, on-site small tests are carried out on the red mud to be treated according to the theoretical calcium sulfate/red mud ratio and the magnesium chloride/red mud ratio obtained in the example 2 and by combining the results of measuring the content of gypsum in the flue gas desulfurization slag, the content of magnesium ions in bittern and the water content of the red mud. On the basis, in consideration of the complexity of field construction, such as the space-time variability of alkalinity in the red mud to be treated, the uncertainty of the mixing degree of the treating agent and the red mud, the limitation of reaction time and the like, the proportion of the treating agent and the red mud needs to be increased so as to ensure that the preset treatment target is achieved. The following illustrates how this method is applied, taking the red mud at the location of sample 2 as an example:
the content of gypsum in the flue gas desulfurization slag is directly measured by using an X-ray fluorescence spectrometer (XRF) and an X-ray diffractometer (XRD). The used flue gas desulfurization slag is estimated to contain about 77% of gypsum.
The purity of magnesium chloride in bittern was determined using inductively coupled plasma optical emission spectroscopy (ICP-OES) instrument or atomic absorption spectroscopy (ASS). The bittern used was measured to contain 66.8 g/l magnesium ions, converted to 566 g/l magnesium chloride hexahydrate.
Measuring the water content of the red mud: taking about 10 g of fresh red mud (accurate to 0.01 g) in a 50 ml glass beaker, drying the red mud in an oven controlled at 105 ℃ until the weight of the red mud is constant, and calculating the water content of the red mud by the following formula:
the water content (%) of red mud is (weight of fresh red mud-weight of dried red mud)/weight of fresh red mud x 100
The water content of the red mud to be treated is measured to be 36 percent.
8. 50 g of fresh red mud (converted into 32 g of dried red mud) is placed in a 150 ml beaker, and 3 g of flue gas desulfurization residue (32 g x 0.07/0.77), 1ml of bittern (about 0.57 g of magnesium chloride) and 125ml of water are added
After mixing, the suspension was stirred for 30 minutes on a magnetic stirrer and the pH of the suspension was determined to be 8.87.
9. The steps for treating the red mud of about 40 tons on site are as follows: mixing the red mud and water of about 125 cubic meters to form slurry, conveying the slurry into a first-stage reaction tank, adding 1.25 cubic meters of bittern, stirring for half an hour, adding 3 tons of flue gas desulfurization residues, and continuously stirring for half an hour in a stirring tank to obtain a suspension with the pH value of 7.75. The treated mud is then fed to a filter press, the red mud is conveyed to a yard after being dried by pressing, and the pressed water is recycled (see figure 3).
And (3) comparison test:
in patent No. 200410085439.5, a method for planting grass in a dry-discharging red mud yard is mentioned that a mode of reducing the alkalinity of red mud by simply using brine is an early technology for harmless treatment of red mud in the team, compared with the technology, the flue gas desulfurization slag and the stirring system additionally added in the invention can not only improve the speed of reducing the pH value of the red mud, but also reuse a solid waste on the premise of not increasing the additional treatment cost, and the contrast effect of the two technologies is as follows:
according to the treatment technology in patent number 200410085439.5 of a method for planting grass in a dry-discharging red mud yard, 50 g of fresh red mud is placed in a 150 ml beaker, 125ml of water is added, the mixture is stirred for 1 hour, 1ml of bittern is added, the mixture is static, the pH value of the suspension is 9.47 after 30 minutes of measurement, the pH value of the suspension is 9.12 after 1 hour, and the pH value of the suspension is 8.91 after 2 hours.
| Raw material | The invention | Patent' method for planting grass in dry-discharge red mud yard |
| Flue gas desulfurization slag | 3g | - |
| Bittern | 1ml | 1ml |
| Water (I) | 125ml | 125ml |
| Red mud | 50g | 50g |
The results are compared as follows:
| alkaline neutralizing effect | The invention | Patent' method for planting grass in dry-discharge red mud yard |
| 30min | 8.87 | 9.47 |
| 1h | 8.47 | 9.12 |
| 2h | 8.09 | 8.91 |
According to component determination, the content of MgCl2 in the bittern reaches 60%, as MgCl2 belongs to soluble salt, the salinity of red mud is easily too high after the red mud is added, and the growth of subsequent vegetation is not facilitated, according to the measurement and calculation, 1ml of bittern is added into 125ml of red mud solution, the content of MgCl2 is 0.48%, most saline-alkali tolerant plants have the tolerable soil salinity range of 0.3% -0.4%, and the result exceeds the concentration, so the bittern is not easily added too much. 1ml of bittern is already the upper limit of the amount added.
Claims (3)
1. An optimization method for performing harmless treatment on red mud which is industrial waste residue by using easily obtained industrial waste is characterized by comprising the following specific steps of:
raw materials: red mud, flue gas desulfurization slag and bittern;
a. measuring the content of gypsum in the flue gas desulfurization slag, measuring the content of magnesium ions in bittern, and converting into magnesium chloride hexahydrate;
b. and (3) measuring the alkalinity of the red mud water extract:
adding 10 g of dried red mud into 50 ml of deionized water, oscillating on an oscillator for 1 hour, taking 25ml of extracting solution, continuously titrating the 25ml of extracting solution by using 0.05M HCl solution until the end point pH =7, and obtaining the alkalinity of the water extracting solution of the red mud by using the following formula according to the volume of the consumed HCl solution:
alkalinity (millimole/kg) = 2v × 0.05 × 100 = 10v of the red mud water extract; wherein v is the number of milliliters of HCl solution consumed by titrating the red mud water extract;
c. the method for measuring the total alkalinity of the red mud comprises the following steps:
taking 10 g of dried red mud, adding 20 ml of 0.05M hydrochloric acid solution to obtain red mud suspension, continuously titrating the red mud suspension by using 0.05M HCl solution until the pH of the final point is =7, and obtaining the total alkalinity of the red mud by using the following formula according to the volume of the consumed HCl solution:
total alkalinity (millimole/kg) = (v +20) × 0.05 × 100 = (v +20) × 5 of red mud
In the above formula, v is the number of milliliters of HCl solution consumed by titrating the red mud suspension;
d. method for removing OH in red mud by calcium sulfate - Capacity of (mmol/kg) =1000/86 ×1000 = 11627；
The weight ratio of calcium sulfate to red mud = total alkalinity of red mud/11627, according to the value range of the weight ratio of calcium sulfate to red mud of the dose-response experiment, adding calcium sulfate according to different weight ratios of calcium sulfate to red mud, then continuously monitoring the pH of the reaction solution, and determining the addition ratio of the pure gypsum required for reducing the pH of the red mud to below 9, namely the actual weight ratio of calcium sulfate dihydrate to red mud, wherein the detection time is 10, 25 and 50 hours after the test is started, and if the pH is not reduced to below 9 after 50 hours, the pH is measured again every 25 hours until the pH is reduced to below 9;
e. method for removing OH in red mud by magnesium chloride - Capacity of (mmol/kg) = 1000/101.5 × 1000 = 9852
Magnesium chloride hexahydrate/red mud weight ratio = alkalinity of red mud water extract/9852
f. Carrying out comprehensive analysis and determining the weight ratio of magnesium chloride to calcium sulfate during red mud treatment to be
Mixing the magnesium chloride/red mud ratio: the actual calcium sulfate/red mud weight ratio = the weight ratio of magnesium chloride/calcium sulfate;
then determining the dosage of bittern and flue gas desulfurization slag when treating the red mud according to the content of gypsum in the flue gas desulfurization slag and the content of magnesium chloride in the bittern;
g. measuring the water content of the red mud, calculating the mass of the dried red mud converted from the fresh red mud, and calculating the use amounts of the flue gas desulfurization slag and the bittern according to the mass of the actual dried red mud, the weight ratio of calcium sulfate dihydrate to the red mud, the weight ratio of magnesium chloride hexahydrate to the red mud, the content of gypsum in the flue gas desulfurization slag and the content of magnesium chloride hexahydrate in the bittern;
h. inputting the red mud into a reaction tank, and mixing the raw materials according to the weight ratio of the red mud: adding water according to the weight ratio of 1:2.5, adding the dosage of bittern and flue gas desulfurization slag determined in the step g, stirring, inputting the slurry into a filter press, conveying the squeezed red mud to a storage yard, and recycling the squeezed water.
2. The optimization method according to claim 1, wherein the determination of the content of gypsum in the flue gas desulfurization slag is performed by direct determination using an X-ray fluorescence spectrometer and an X-ray diffractometer.
3. The optimization method of claim 1, wherein the determination of the content of magnesium ions in the bittern is performed by using inductively coupled plasma optical emission spectrometer or atomic absorption spectrometer.
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