CN115072742A - Efficient recovery method of potassium in potassium-containing tail salt - Google Patents
Efficient recovery method of potassium in potassium-containing tail salt Download PDFInfo
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- CN115072742A CN115072742A CN202210797875.3A CN202210797875A CN115072742A CN 115072742 A CN115072742 A CN 115072742A CN 202210797875 A CN202210797875 A CN 202210797875A CN 115072742 A CN115072742 A CN 115072742A
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Abstract
The invention relates to the technical field of chemical detection, in particular to a method for efficiently recovering potassium in potassium-containing tail salt, which comprises the steps of adding fresh water to tail salt piled up for a long time after potassium flotation of carnallite raw ore for washing, and carrying out secondary washing on a solid phase after solid-liquid separation by using raw halogen; and mixing the two liquid phases, adding brine by using old brine, and naturally evaporating to recycle potassium chloride in the long-term stacked tail salt. Wherein, the brine amount entering the salt pan evaporation stage after washing is higher than that of other processes, the brine amount required by the salt pan evaporation is less, the required area of the salt pan is less, and the operation of the salt pan is easier to control. The recovery rate of KCl of the brine-blending completion liquid can reach 85 percent, and the comprehensive recovery rate of KCl can reach 73.22 percent; the final product carnallite is more beneficial to the production of a flotation workshop.
Description
Technical Field
The invention relates to the technical field of chemical detection, in particular to a high-efficiency recovery method of potassium in potassium-containing tail salt.
Background
The tail salt heap is produced and discharged in a potash fertilizer workshop, the potassium chloride content in tail solids discharged in daily production is about 1%, tail liquid with high potassium content (the potassium chloride content in carnallite saturated liquid is 3.7-4.4%) is discharged into a tailing area while the tail solids are discharged into the tailing area, the carnallite saturated mother liquid has the phenomenon of evaporation and water loss in the long-term stacking process of the tail salt, the mother liquid evaporates and loses water to crystallize carnallite, and finally, the potassium chloride content in the tail salt stacked in the tailing area reaches 3% except a large amount of sodium salts. However, the tail salt has too low potassium content and too high sodium content, so that the tail salt cannot be recycled by a forward flotation process and a reverse flotation process, and can only be stacked for a long time, and low potassium resources are left unused.
At present, the potassium in the tail salt containing potassium in the salt lake region is recovered mainly by washing the tail salt, so that the potassium in the tail salt is converted into liquid potassium from solid potassium, and then the liquid phase is evaporated to obtain solid (carnallite) with high potassium content, so that the solid can be recovered and utilized, and the main difference of each process lies in the preparation of a washing solution. But no further study was made to recover potassium entrained in the washed solids.
Disclosure of Invention
In order to solve the technical problem, potassium chloride crystallized and separated from tail salt piled for a long time after carnallite raw ore is subjected to potassium flotation is recycled through two-step washing, so that the potassium recovery rate is improved. Aims to provide a method for efficiently recovering potassium in potassium-containing tail salt.
The invention discloses a method for efficiently recovering potassium in potassium-containing tail salt, which specifically comprises the following steps:
step 1, crushing tail salt, adding fresh water with the tail salt content of 20-25%, stirring and washing for 5-30 min;
step 3, adding old brine with the tail salt content of 10-50% into the two liquid phases for brine blending to obtain brine blending completion liquid;
and 4, evaporating the brine-blending completion liquid, and then carrying out compound analysis on the obtained substances (carnallite and old brine).
Further, in the step 1, the amount of the added fresh water is 22% of the amount of the tail salt, and the washing time is 20 min; stirring with JJ-1 electric stirrer.
Further, in the step 1, the tail salt is a tail salt stacked for a long time after the carnallite raw ore is subjected to potassium flotation, wherein the content of potassium chloride separated by crystallization is 3%.
Further, in the step 2, a centrifugal machine is adopted for solid-liquid separation, and the centrifugal speed is 800 r/min; the amount of the added original halogen is 40% of the amount of the tail salt.
Further, in the step 3, the amount of the old brine added is 40% of the amount of the tail salt.
Furthermore, in the step 4, the evaporation time is determined by the total amount of the brine-blending completion liquid and the evaporation area, and compared with other processes which only have a carnallite evaporation stage and no halite evaporation stage, the method needs less area of a salt pan and less evaporation amount.
Compared with the prior art, the invention has the following beneficial effects:
the method comprises the steps of adding fresh water into tail salt piled up for a long time after potassium flotation of carnallite raw ore to wash, and performing secondary washing on solid phase after solid-liquid separation by using raw brine; and mixing the two liquid phases, adding brine by using old brine, and naturally evaporating to recycle potassium chloride in the long-term stacked tail salt. Wherein, the brine amount entering the salt pan evaporation stage after washing is higher than that of other processes, the brine amount required by the salt pan evaporation is less, the required area of the salt pan is less, and the operation of the salt pan is easier to control. The recovery rate of KCl of the brine-blending completion liquid can reach 85 percent, and the comprehensive recovery rate of KCl can reach 73.22 percent; the final product carnallite is more beneficial to the production of a flotation workshop
Drawings
FIG. 1 is a process flow diagram of the method of the present invention;
FIG. 2 is a diagram of the analytical phase of the tail salt washing theory of the present invention;
FIG. 3 is a phase diagram at 10 ℃;
FIG. 4 is a graph showing the relationship between washing time and the amount of potassium chloride in a solid phase;
FIG. 5 is a phase diagram of old brine washing at 20 ℃;
FIG. 6 is a phase diagram of 20 ℃ washing of the crude halide;
FIG. 7 is a graph showing the relationship between the amount of the original halogen added and the amount of potassium chloride in the washing solid phase;
FIG. 8 is an enlarged phase diagram (10 ℃ C.) of the test materials;
FIG. 9 is a phase diagram of the evaporation route at 10 ℃;
FIG. 10 is a graph showing the variation of KCl in the naturally evaporated liquid phase of brine.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
1. Theoretical basis
(1) Tail salt composition analysis
The composition of tail salt discharged in potash fertilizer workshop production completely meets the requirements of workshop process indexes, the content of potassium chloride in the tail salt of the tail salt pile is higher than that of tail salt potassium chloride discharged in the workshop because the mother liquor discharged in the workshop production is carnallite saturated liquor, wherein the content of potassium chloride is 3.7-4.4%, the carnallite saturated mother liquor has the phenomenon of evaporation and dehydration in the long-term stacking process of the tail salt, the mother liquor evaporates and dehydrates to crystallize carnallite, and the potassium chloride content of the salt tail in the stacking process reaches 3%. The research object of the invention is to recycle the potassium chloride crystallized and precipitated from the long-term stacked tail salt.
Theoretical analysis according to the phase diagram (fig. 2): adding a proper amount of water into tail salt (4 points) containing about 3 percent of potassium chloride to dissolve the tail salt to ensure that the liquid phase point reaches the saturation point (1 point) of sylvite, adding original bittern (3 points) or old bittern (6 points) into the separated liquid phase, controlling the point of adding bittern to be above (2 points) or (5 points) (the saturation point of the potassium chloride passes through the sylvite precipitation stage (E point)), and evaporating the tail salt by solarization of a salt field to precipitate carnallite to be recovered.
Washing operation: tail salt (point 4) + water-sodium salt solidus point + wash solution (point 1);
original halogen blending operation: adding the cleaning solution (1 point) and the original halogen (3 points) into the original halogen mixed halogen solution (2 points);
old brine mixing operation: adding the cleaning solution (1 point) and the old brine (6 points) into the brine-mixed solution (5 points);
dot description in the phase diagram:
point 1: adding water into the tail salt to wash the tail salt, and then putting the potassium-containing brine into position points in a phase diagram;
point 2: adding water into tail salt for washing, mixing potassium-containing brine and raw brine through brine mixing operation, and mixing brine at positions in a phase diagram;
point 3: the position point of the original halogen in the phase diagram;
point 4: position points of the tail salt in the phase diagram;
point 5: adding water into tail salt for washing, mixing potassium-containing brine and old brine through brine mixing operation, and mixing brine at positions in a phase diagram;
point 6: the position point of the old brine in the phase diagram;
point E: the location point of the carnallite and sylvine saturation point in the phase diagram;
(2) research thought
The tail salt contains more than 3 percent of potassium chloride, fresh water is added to the tail salt to dissolve the tail salt so that the tail salt enters a liquid phase, then the liquid phase is evaporated and separated out in a carnallite form to be recycled, and according to a phase diagram and a dissolution theory, the optimal composition point of the washed liquid phase is on a potassium-sodium saturation line in the phase diagram; the potassium content in the liquid phase after washing is higher, so that the potassium content in the mother liquor carried by the solid phase after washing is higher, the recovery rate is reduced, and the recovery rate can be improved by reducing the potassium content in the mother liquor carried by the solid phase after washing under the condition that the whole mother liquor carrying amount is not changed, so that the liquid phase with the lower potassium content is used for secondary washing in the project implementation process to exchange the mother liquor with the high potassium content to improve the recovery rate.
2. Determining the amount of washing water
(1) The purpose is as follows: the best washing water consumption is determined by comparing the KCl dissolution effect of the tail salt after washing under different washing water quantities through experiments under the condition of unchanged washing stirring intensity and washing time.
(2) The instrument comprises the following steps: JJ-1 electric stirrer, JR-150/450 dehydration sample machine.
(3) The process is as follows: weighing tail salt (1.00kg) with the same weight in a 3000ml beaker, adding fresh water with different weights, stirring for 5min under the same stirring strength, and separating by a centrifuge.
The optimal water amount (potassium is converted into liquid phase after tail salt washing) of the tail salt added with water of the company is calculated to be 22% by theory, and the washing effect is examined by adding different amounts of fresh water in the test process for the same stirring time.
Table 1 washing water quantity determination test table (fixed washing time)
The experiment analysis can obtain that when the water addition amount is 90% of the theoretical value, KCl in the tail salt is not completely dissolved, when the water addition amount is 110% of the theoretical value, KCl is completely transferred into a liquid phase, the amount of NaCl dissolved in the liquid phase is increased along with the increase of the water addition amount, the area of a sodium salt field required in the subsequent evaporation of the salt field is increased, along with the increase of the washing water amount, a liquid phase point is further away from a saturation line and approaches to a pure sodium salt point, the sodium salt dissolution is increased along with the increase of the water amount, the recovery effect on potassium is avoided, and the washing water amount is comprehensively analyzed to be the theoretical water addition amount (figure 3).
3. Determination of washing time
(1) The purpose of the test is as follows: under the condition of unchanged washing stirring intensity and washing water quantity, the best washing time is determined by comparing the dissolving effect of KCl after tail salt is washed under different washing times through tests.
Table 2 washing time determination test table (fixed water addition amount)
(2) And (4) conclusion: the test determines that the washing time is 20min, the carnallite in the tail salt is dissolved completely to meet the test requirement, and the effect is best (see the attached figure 4 for details).
3. Secondary washing and brine adding test
(1) The purpose of the test is as follows: the secondary washing water quantity (reducing the entrainment of the mother liquor) and the brine addition are determined, and the low-potassium sodium saturated mother liquor is used for replacing the high-potassium liquid entrained in the solid phase after the fresh water washing so as to improve the recovery rate, so that the raw material is finally tested by respectively using the original brine and the old brine as the secondary washing liquid.
TABLE 3 secondary washing and brine addition analysis results Table
(2) Summary of the test: the old brine washing test shows that the KCl content in the washing liquid phase is reduced by simultaneously adding fresh water and old brine washing, the KCl content (0.79%) carried in the washing solid phase is lower than that (0.91%) washed by only adding fresh water, and the recovery rate of KCl in the process can be improved. The original halogen washing test shows that the KCl content in the solid phase is reduced more obviously (0.28%) than that in the one-step washing after the washing process is divided into two steps. However, the amount of the original halogen is large, and the operation in industrial production is difficult. The secondary washing operation further improved the recovery (FIGS. 5 and 6).
TABLE 4 analysis results of two washing times (reduction of entrainment of mother liquor)
(3) The best test results are obtained when the washing amount of the secondary raw brine is 40% of that of the tail salt (see the attached figure 7 for details).
4. Enlargement test
(1) The purpose of the test is as follows: and carrying out an expansion test by using the process parameters determined by the laboratory test, and examining the reproducibility of the result. And adding fresh water into the tail salt to wash the solid-liquid separation, and washing the washed solid phase for the second time by using the original halogen.
TABLE 5 Primary brine Secondary Wash analysis results Table
Note: recovery rate (KCl metallicity in halogen-original halogen-KCl metallicity in old halogen)/KCl metallicity in tail salt
Calculating according to the group of test data, 10% of KCl residue in the finally discharged and washed solid 2 is discharged, the leakage and drip loss in the operation process is about 4%, and the final loss rate of KCl is about 3.21%; the KCl yield in the washing process is 85.82 percent, and the KCl recovery rate required in the washing process is achieved (figure 8).
(2) The test summary is as follows: and determining process parameters according to the lab test, and reproducing the lab test result through an expansion test.
5. Test of natural evaporation
(1) The purpose of the test is as follows: and naturally evaporating the liquid phase after washing to obtain technological parameters of each stage of the evaporation process.
The natural evaporation test was carried out in 7 groups in total at different weights (brine level), and the specific evaporation test was carried out at the same time. In the test process, the total water amount of the No. 3 test is small (32.45kg), the separation operation is not carried out in the early stage of the evaporation process, and only the analysis of the liquid phase component test is carried out to guide the rest evaporation tests according to the result.
Test No. 3: the total water amount is small, the separation operation is not carried out in the early stage of the evaporation process, and only the liquid phase component assay analysis is carried out to guide other evaporation tests.
Table 63 evaporation test analysis results table
Test No. 7:
table 77 evaporation test analysis results table
Naturally evaporating the material
TABLE 8 Natural evaporation material balance table
(2) The purpose of the test is as follows: in the experiment implementation process, the water running time in the salt pan is long when the salt pan is evaporated finally, and the old brine added in the brine-blending operation is 80% of the theoretical value, so that the brine in the salt pan reaches a saturation point when reaching a carnallite pool without separating out carnallite in a regulating pool, and the recovery rate in the whole evaporation process is 85.32%. Taking gelmu area as an example, the annual net evaporation capacity is 3000mm, the annual evaporation capacity of a salt pan system is 4200 × 38.28 ═ 160776(t) calculated according to 40 ten thousand tons of annual treated tail salt, and 20272(t) stage evaporation of sodium salt requires 9184m sodium salt pan 2 The carnallite pool 106442m is needed for the carnallite stage evaporation 140504(t) 2 . The carnallite pool is divided into two blocks which need 140% of theoretical value, namely 149019m, due to uncertain factors such as ore removal and the like 2 Total 158203m of salt pan 2 。
6. Summary of the invention
The secondary washing of the tail salt can effectively reduce the solid-phase entrainment amount after washing, and the recovery rate of the whole process is improved compared with other processes. The brine entering the salt pan evaporation stage after washing has higher content of potassium than other processes, the brine needing evaporation in the salt pan has less brine amount, the required area of the salt pan is less, and the operation of the salt pan is easier to control.
The technical parameters of each operation section are determined through condition tests: the washing water amount (22% of the tail salt amount), the fresh water washing time (20min), the original bittern washing amount (40% of the tail salt amount) and the old bittern mixing amount (40% of the tail salt amount).
Example 2
A method for efficiently recovering potassium in potassium-containing tail salt specifically comprises the following steps:
step 1, crushing tail salt (tail salt piled for a long time after carnallite raw ore is subjected to potassium flotation, wherein the content of potassium chloride separated out by crystallization is 3%), adding fresh water with the tail salt content of 22% to wash and dissolve the potassium chloride in the tail salt, and washing for 20 min;
step 3, adding old brine with the tail salt content of 40% into the two liquid phases for brine blending to obtain brine blending completion liquid;
step 4, evaporating the brine-blending completion liquid, and carrying out compound analysis on the obtained substances (carnallite and old brine); the fermentation time is determined by the total amount of brine-blending completion liquid and the evaporation area, and compared with other processes which only have a carnallite evaporation stage and no halite evaporation stage, the method has the advantages of less required area of a salt field and less evaporation amount.
By taking the Keohan salt lake group, the Meghai salt lake Zhonghang group and the Qiqianghospital salt lake company as examples, the potassium-containing tail salt mine utilization comparison shows that:
TABLE 9 comparison table of utilization of potassium-containing tailings
Through the process route and the comparative analysis result of the designed washing scheme, the recovery rate of KCl of the brine-blending completion liquid prepared by the method can reach 85 percent, the comprehensive recovery rate of KCl can reach 73.22 percent, and the design requirement is met.
Example 3
A method for efficiently recovering potassium in potassium-containing tail salt specifically comprises the following steps:
step 1, crushing tail salt (tail salt piled for a long time after carnallite raw ore is subjected to potassium flotation, wherein the content of potassium chloride separated out by crystallization is 3%), adding fresh water with 20% of tail salt amount to wash and dissolve the potassium chloride in the tail salt, and washing for 25 min;
step 3, adding old brine with the tail salt content of 45% into the two liquid phases for brine blending to obtain brine blending completion liquid;
step 4, evaporating the brine-blending completion liquid, and carrying out compound analysis on the obtained substances (carnallite and old brine); the evaporation time is determined by the total amount of brine-blending completion liquid and the evaporation area, and compared with other processes which only have a carnallite evaporation stage and do not have a rock salt evaporation stage, the method has the advantages of small required area of a salt field and small evaporation amount.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The method for efficiently recovering potassium in potassium-containing tail salt is characterized by comprising the following steps:
step 1, crushing tail salt, adding fresh water with the tail salt content of 20-25%, stirring and washing for 5-30 min;
step 2, carrying out solid-liquid separation on the washing liquid obtained in the step 1, and collecting a liquid phase; adding original bittern with tail salt content of 10-50% into the solid phase, washing for 5-10min, collecting and combining the two liquid phases;
step 3, adding old brine with the tail salt content of 10-50% into the two liquid phases for brine blending to obtain brine blending completion liquid;
and 4, evaporating the brine-blending completion liquid, and then carrying out compound analysis on the obtained substance.
2. The method for efficiently recovering the potassium in the potassium-containing tail salt according to claim 1, wherein in the step 1, the amount of fresh water added is 22 percent of the amount of the tail salt, and the washing time is 20 min; stirring with JJ-1 electric stirrer.
3. The method for efficiently recovering potassium in potassium-containing tail salt according to claim 1, wherein in the step 1, the tail salt is the tail salt piled up for a long time after carnallite raw ore is subjected to potassium flotation, and the content of crystallized potassium chloride is 3%.
4. The method for efficiently recovering the potassium in the potassium-containing tail salt according to claim 1, wherein in the step 2, a centrifugal machine is adopted for solid-liquid separation, and the centrifugal speed is 800 r/min; the amount of the original halogen added is 40% of the amount of the tail salt.
5. The method for efficiently recovering potassium in potassium-containing tail salt according to claim 1, wherein in the step 3, the amount of the old brine added is 40% of the amount of the tail salt.
6. The method as claimed in claim 1, wherein in the step 4, the evaporation time is determined by the total amount of the brine-blending completion liquid and the evaporation area.
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