CN114477250B - Method for preparing magnesium sulfate by utilizing anthraquinone waste acid - Google Patents
Method for preparing magnesium sulfate by utilizing anthraquinone waste acid Download PDFInfo
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- CN114477250B CN114477250B CN202210088896.8A CN202210088896A CN114477250B CN 114477250 B CN114477250 B CN 114477250B CN 202210088896 A CN202210088896 A CN 202210088896A CN 114477250 B CN114477250 B CN 114477250B
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- Prior art keywords
- magnesium sulfate
- mother liquor
- purified
- waste acid
- sulfuric acid
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- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 title claims abstract description 164
- 229910052943 magnesium sulfate Inorganic materials 0.000 title claims abstract description 82
- 235000019341 magnesium sulphate Nutrition 0.000 title claims abstract description 82
- 239000002699 waste material Substances 0.000 title claims abstract description 32
- 239000002253 acid Substances 0.000 title claims abstract description 29
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 150000004056 anthraquinones Chemical class 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000012452 mother liquor Substances 0.000 claims abstract description 60
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000013049 sediment Substances 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 21
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000013078 crystal Substances 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000012535 impurity Substances 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 18
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 16
- 239000010802 sludge Substances 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000002425 crystallisation Methods 0.000 claims abstract description 12
- 230000008025 crystallization Effects 0.000 claims abstract description 12
- 239000012065 filter cake Substances 0.000 claims abstract description 12
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000010413 mother solution Substances 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 abstract description 8
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000012047 saturated solution Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- SJEBAWHUJDUKQK-UHFFFAOYSA-N 2-ethylanthraquinone Chemical compound C1=CC=C2C(=O)C3=CC(CC)=CC=C3C(=O)C2=C1 SJEBAWHUJDUKQK-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/40—Magnesium sulfates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method for preparing magnesium sulfate by utilizing anthraquinone waste acid, which comprises the following steps: standing and separating anthraquinone waste acid to obtain dilute sulfuric acid solution and sediment; mixing dilute sulfuric acid solution, magnesium oxide and 98wt% concentrated sulfuric acid to react to obtain a solid-liquid mixture; carrying out solid-liquid separation on the solid-liquid mixture to obtain magnesium sulfate mother liquor and a filter cake; sequentially carrying out heating concentration, cooling crystallization and centrifugal separation on the magnesium sulfate mother solution to obtain mother solution to be purified and magnesium sulfate crystals; adding an organic extractant into the mother liquor to be purified to adsorb impurities, and separating to obtain sludge sediment and purified mother liquor; returning the purified mother liquor to the concentration stage; the method is simple and easy to implement, and can realize the sedimentation of impurities only by adding an organic extractant, thereby realizing the recycling of mother liquor, improving the utilization rate of waste acid and realizing the maximization of economy.
Description
Technical Field
The invention relates to the technical field of waste acid recycling, in particular to a method for preparing magnesium sulfate by utilizing anthraquinone waste acid.
Background
At present, a large amount of waste sulfuric acid is generated in the production process of 2-ethyl anthraquinone, sludge-containing sediments in the waste sulfuric acid cannot be recycled, direct discharge needs to be treated, energy consumption is overlarge, and waste of dilute sulfuric acid components in waste acid can be caused.
The traditional treatment mode is that magnesium sulfate is prepared by waste acid, magnesium sulfate mother liquor after crystallization in the magnesium sulfate preparation process is generally returned to a front-end process as circulating liquid for production, sludge sediment (in the form of particles) in the magnesium sulfate mother liquor is continuously accumulated in the production process, the concentration and crystallization effects are finally affected, the yield is reduced, and the magnesium sulfate mother liquor is discharged or replaced after impurities are accumulated to a certain extent; because of the continuous accumulation of impurities, a large amount of bubbles can be generated in the concentration process and are black small particles, the traditional treatment mode is realized through secondary crystallization, but the magnesium sulfate mother liquor is in excessive impurity content in the magnesium sulfate mother liquor during secondary crystallization, the size of magnesium sulfate crystal particles is uneven, black particles are also carried, and separation is realized through a scraper centrifuge, so that the whole process flow is prolonged, and the magnesium sulfate mother liquor obtained through secondary crystallization cannot be circulated in an infinite way and needs to be discharged periodically.
Disclosure of Invention
Aiming at the problem that the magnesium sulfate mother liquor increases along with the increase of the cycle times, and the impurity enrichment reduces the quality of magnesium sulfate products, the invention provides a method for preparing magnesium sulfate by utilizing anthraquinone waste acid.
The technical scheme of the invention is as follows: a method for preparing magnesium sulfate by utilizing anthraquinone waste acid comprises the following steps:
standing and separating anthraquinone waste acid to obtain dilute sulfuric acid solution and sediment;
mixing dilute sulfuric acid solution, magnesium oxide and 98wt% concentrated sulfuric acid to react to obtain a solid-liquid mixture;
Carrying out solid-liquid separation on the solid-liquid mixture to obtain magnesium sulfate mother liquor and a filter cake;
Sequentially carrying out heating concentration, cooling crystallization and centrifugal separation on the magnesium sulfate mother solution to obtain mother solution to be purified and magnesium sulfate crystals;
Adding an organic extractant into the mother liquor to be purified to adsorb impurities, and separating to obtain sludge sediment and purified mother liquor;
The purified mother liquor is returned to the concentration stage.
Further defined, the sediment is subjected to solid-liquid separation through a vacuum drum suction filter, wherein filtrate is returned to the mixing reaction stage of the dilute sulfuric acid solution, magnesium oxide and 98wt% of concentrated sulfuric acid, and filter residues are sent out.
Further defined, the organic extractant is added in an amount of less than 5% by mass of the mother liquor to be purified.
Further limiting, adding magnesium sulfate crystals in the heating concentration stage, and stopping heating when the Baume degree of the magnesium sulfate mother solution is more than or equal to 41.
Further defined, the Baume degree of the magnesium sulfate mother liquor at the end of the cooling crystallization stage is less than or equal to 31.
Further limited, in the cooling crystallization stage, the magnesium sulfate mother liquor after heating and concentrating is cooled by adopting a water-proof cooling mode.
Further defined, during the heat concentration stage, the magnesium sulfate crystals are melted by adding superheated steam.
Further defined, in the heating concentration stage, the temperature of the magnesium sulfate mother liquor is 70-80 ℃. The beneficial effects of the invention are as follows:
1. According to the invention, the organic extractant is added, so that the mass of the impurities in the mother liquor to be purified is increased after adsorption, and the impurities are settled and accumulated to form sludge sediments, thereby achieving the layering purpose, the sludge sediments can be removed by filtering, the purified mother liquor is returned to be continuously utilized, the problems that the magnesium sulfate solution cannot be recycled due to enrichment of the organic impurities and is required to be discharged and treated are solved, the purity requirement of raw magnesium oxide is reduced, the recovery rate of magnesium sulfate is improved, and the environmental pollution is reduced.
2. The invention adopts the vacuum drum suction filter to filter the sediment, the process can be continuously carried out, less manpower is required, and the filtrate in the filter residue can be recycled, so the treatment efficiency is high and the manpower cost is saved.
Drawings
Fig. 1 is a flowchart of example 1.
Detailed Description
Example 1
In this example, the concentration of the dilute sulfuric acid solution was 50wt%.
As shown in fig. 1, a method for preparing magnesium sulfate by using anthraquinone waste acid comprises the following steps:
S1, introducing anthraquinone waste acid into a physical sedimentation tank, standing and separating to obtain dilute sulfuric acid solution and sediment, wherein in the step, the total number of the physical sedimentation tanks is two, and one is used for standby;
S2, carrying out solid-liquid separation on the sediment through a vacuum drum suction filter, wherein filtrate is returned to a dilute sulfuric acid solution, and a filter cake is sent out;
s3, mixing and reacting the dilute sulfuric acid solution, the magnesium oxide and 98wt% of concentrated sulfuric acid to obtain a solid-liquid mixture, carrying out solid-liquid separation on the solid-liquid mixture to obtain magnesium sulfate mother liquor and a filter cake, and sending the filter cake out;
S4, heating the magnesium sulfate mother liquor by adopting superheated steam, adding magnesium sulfate crystals to form a magnesium sulfate saturated solution, and stopping heating when the temperature of the magnesium sulfate mother liquor is 80 ℃ and the Baume degree reaches 41 during concentration;
S5, after concentration is completed, placing the magnesium sulfate mother liquor into a flowing water bath for cooling, stopping cooling when the temperature of the magnesium sulfate mother liquor is reduced to 30 ℃, and performing solid-liquid separation when the Baume degree is 31 to obtain mother liquor to be purified and magnesium sulfate crystals, and drying the magnesium sulfate crystals;
and S6, adding an organic extractant into the mother liquor to be purified, adsorbing organic impurities, increasing the mass, settling and accumulating to form sludge sediment, separating the sludge sediment from a liquid phase, separating to obtain the purified mother liquor and the sludge sediment, and returning the mixed purified mother liquor to the step S4.
Example 2
In this example, the concentration of the dilute sulfuric acid solution was 40wt%.
A method for preparing magnesium sulfate by utilizing anthraquinone waste acid comprises the following steps:
S1, introducing anthraquinone waste acid into a physical sedimentation tank, standing and separating to obtain dilute sulfuric acid solution and sediment, wherein in the step, the total number of the physical sedimentation tanks is two, and one is used for standby;
S2, carrying out solid-liquid separation on the sediment through a vacuum drum suction filter, wherein filtrate is returned to a dilute sulfuric acid solution, and a filter cake is sent out;
s3, mixing and reacting the dilute sulfuric acid solution, the magnesium oxide and 98wt% of concentrated sulfuric acid to obtain a solid-liquid mixture, carrying out solid-liquid separation on the solid-liquid mixture to obtain magnesium sulfate mother liquor and a filter cake, and sending the filter cake out; s4, heating the magnesium sulfate mother liquor by adopting superheated steam, adding magnesium sulfate crystals to form a magnesium sulfate saturated solution, concentrating the magnesium sulfate mother liquor at the temperature of 80 ℃, and stopping heating when the Baume degree of the magnesium sulfate mother liquor is 45;
s5, after concentration is completed, placing the magnesium sulfate mother liquor into a flowing water bath for cooling, stopping cooling when the temperature of the magnesium sulfate mother liquor is reduced to 20 ℃, and performing solid-liquid separation when the Baume degree is 20 to obtain mother liquor to be purified and magnesium sulfate crystals, and drying the magnesium sulfate crystals;
and S6, adding an organic extractant into the mother liquor to be purified, adsorbing organic impurities, increasing the mass, settling and accumulating to form sludge sediment, separating the sludge sediment from a liquid phase, separating to obtain the purified mother liquor and the sludge sediment, and returning the mixed purified mother liquor to the step S4.
Example 3
In this example, the concentration of the dilute sulfuric acid solution was 40wt%.
A method for preparing magnesium sulfate by utilizing anthraquinone waste acid comprises the following steps:
S1, introducing anthraquinone waste acid into a physical sedimentation tank, standing and separating to obtain dilute sulfuric acid solution and sediment, wherein in the step, the total number of the physical sedimentation tanks is two, and one is used for standby;
S2, carrying out solid-liquid separation on the sediment through a vacuum drum suction filter, wherein filtrate is returned to a dilute sulfuric acid solution, and a filter cake is sent out;
s3, mixing and reacting the dilute sulfuric acid solution, the magnesium oxide and 98wt% of concentrated sulfuric acid to obtain a solid-liquid mixture, carrying out solid-liquid separation on the solid-liquid mixture to obtain magnesium sulfate mother liquor and a filter cake, and sending the filter cake out;
S4, heating the magnesium sulfate mother liquor by adopting superheated steam, adding magnesium sulfate crystals to form a magnesium sulfate saturated solution, and stopping heating when the temperature of the magnesium sulfate mother liquor is 80 ℃ and the Baume degree reaches 41 during concentration;
S5, after concentration is completed, placing the magnesium sulfate mother liquor into a flowing water bath for cooling, stopping cooling when the temperature of the magnesium sulfate mother liquor is reduced to 25 ℃, and performing solid-liquid separation when the Baume degree is 15 to obtain mother liquor to be purified and magnesium sulfate crystals, and drying the magnesium sulfate crystals;
and S6, adding an organic extractant into the mother liquor to be purified, adsorbing organic impurities, increasing the mass, settling and accumulating to form sludge sediment, separating the sludge sediment from a liquid phase, separating to obtain the purified mother liquor and the sludge sediment, and returning the mixed purified mother liquor to the step S4.
On one hand, the discharge of magnesium sulfate mother liquor is reduced; on the other hand, the selection range of the magnesia raw material is widened, more magnesia with more impurities can be treated by increasing the amount of the extractant, and magnesia with high content of impurities and magnesia with low content of impurities can be mixed and put into use, and the reasonable ore blending of the effective components is controlled to select.
As can be seen from examples 1-3, the method for preparing magnesium sulfate by utilizing anthraquinone waste acid disclosed by the invention is simple in process, and can realize sedimentation of impurities only by adding an organic extractant, thereby realizing cyclic utilization of mother liquor, improving the utilization rate of waste acid and realizing economic maximization.
The method for preparing magnesium sulfate by utilizing the anthraquinone waste acid disclosed by the invention can be used for treating magnesium oxide with low magnesium oxide content, so that the difficulty in treating low-content magnesium oxide is greatly reduced, and the treatment cost is reduced.
Finally, it should be noted that: the foregoing description is only of the preferred embodiments of the invention and is not intended to limit the scope of the invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The method for preparing the magnesium sulfate by using the anthraquinone waste acid is characterized by comprising the following steps of:
standing and separating anthraquinone waste acid to obtain dilute sulfuric acid solution and sediment;
mixing dilute sulfuric acid solution, magnesium oxide and 98wt% concentrated sulfuric acid for reaction to obtain a solid-liquid mixture;
Carrying out solid-liquid separation on the solid-liquid mixture to obtain magnesium sulfate mother liquor and a filter cake;
Sequentially carrying out heating concentration, cooling crystallization and centrifugal separation on the magnesium sulfate mother solution to obtain mother solution to be purified and magnesium sulfate crystals;
adding an organic extractant into the mother liquor to be purified to adsorb impurities, and separating to obtain sludge sediment and purified mother liquor; the adding amount of the organic extractant is less than 5% of the mass of the mother liquor to be purified;
And returning the purified mother liquor to the concentration stage for circulation to obtain magnesium sulfate crystals.
2. The method for preparing magnesium sulfate by utilizing anthraquinone waste acid according to claim 1, wherein the sediment is subjected to solid-liquid separation by a vacuum drum suction filter, wherein filtrate is returned to the mixing reaction stage of dilute sulfuric acid solution, magnesium oxide and 98wt% of concentrated sulfuric acid, and filter residues are sent out.
3. The method for preparing magnesium sulfate by using anthraquinone waste acid according to claim 1, wherein magnesium sulfate crystals are added in the heating concentration stage, and heating is stopped when the baume degree of the magnesium sulfate mother liquor is not less than 41.
4. The method for preparing magnesium sulfate by utilizing anthraquinone waste acid according to claim 1, wherein the baume degree of the magnesium sulfate mother solution at the end of the cooling crystallization stage is less than or equal to 31.
5. The method for preparing magnesium sulfate by utilizing anthraquinone waste acid according to claim 1, wherein in the cooling crystallization stage, a water-proof cooling mode is adopted to cool the magnesium sulfate mother liquor after heating and concentrating.
6. The method for preparing magnesium sulfate by using anthraquinone waste acid according to claim 5, wherein in the heating and concentrating stage, the magnesium sulfate crystals are melted by adding superheated steam.
7. The method for preparing magnesium sulfate by using anthraquinone waste acid according to claim 6, wherein the temperature of the magnesium sulfate mother liquor is 70-80 ℃ in the heating concentration stage.
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