CN114477250A - Method for preparing magnesium sulfate by using anthraquinone waste acid - Google Patents
Method for preparing magnesium sulfate by using anthraquinone waste acid Download PDFInfo
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- CN114477250A CN114477250A CN202210088896.8A CN202210088896A CN114477250A CN 114477250 A CN114477250 A CN 114477250A CN 202210088896 A CN202210088896 A CN 202210088896A CN 114477250 A CN114477250 A CN 114477250A
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- China
- Prior art keywords
- magnesium sulfate
- mother liquor
- waste acid
- purified
- sulfuric acid
- Prior art date
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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 161
- 229910052943 magnesium sulfate Inorganic materials 0.000 title claims abstract description 79
- 235000019341 magnesium sulphate Nutrition 0.000 title claims abstract description 79
- 239000002699 waste material Substances 0.000 title claims abstract description 34
- 239000002253 acid Substances 0.000 title claims abstract description 30
- 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 25
- 150000004056 anthraquinones Chemical class 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000012452 mother liquor Substances 0.000 claims abstract description 70
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000013049 sediment Substances 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 239000012535 impurity Substances 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 18
- 239000010802 sludge Substances 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 15
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 15
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012065 filter cake Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims description 9
- 230000008025 crystallization Effects 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 abstract description 7
- 125000004122 cyclic group Chemical group 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract 1
- 238000004062 sedimentation Methods 0.000 description 13
- 238000000151 deposition Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 2
- 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
- 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
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
Images
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 using anthraquinone waste acid, which comprises the following steps: standing and separating the anthraquinone waste acid to obtain a dilute sulfuric acid solution and sediments; mixing and reacting dilute sulfuric acid solution, magnesium oxide and 98 wt% 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; heating and concentrating, cooling and crystallizing the magnesium sulfate mother liquor, and performing centrifugal separation to obtain mother liquor to be purified and magnesium sulfate crystals; adding an organic extracting agent 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, the precipitation of impurities can be realized only by adding the organic extractant, the cyclic utilization of the mother liquor is realized, the utilization rate of waste acid is improved, and the economic maximization is realized.
Description
Technical Field
The invention relates to the technical field of waste acid recycling, in particular to a method for preparing magnesium sulfate by using anthraquinone waste acid.
Background
A large amount of waste sulfuric acid is generated in the production process of 2-ethyl anthraquinone at present, the waste sulfuric acid contains sludge and sediment, the sludge and the sediment cannot be recycled, the waste sulfuric acid is directly discharged and needs to be treated, the energy consumption is overlarge, and the waste of dilute sulfuric acid components in the waste acid is also caused.
The traditional treatment mode is that waste acid is utilized to prepare magnesium sulfate, magnesium sulfate mother liquor after crystallization in the magnesium sulfate preparation process is generally used as circulating liquid to return to a front-end process for production, sludge sediments (in a granular form) in the magnesium sulfate mother liquor can be accumulated continuously in the production process, the concentration and crystallization effects are influenced finally, the yield is reduced, and the magnesium sulfate mother liquor must be discharged or replaced after impurities are accumulated to a certain degree; because impurity is constantly accumulated, a large amount of bubbles can be generated in the concentration process and are small black particles, the traditional treatment mode is realized through secondary crystallization, but the secondary crystallization is realized because the impurity content in the magnesium sulfate mother liquor is too much and the particle size of magnesium sulfate crystals is not uniform, black particles are also arranged, and the separation needs to be realized through a scraper centrifuge, so that the whole process flow is lengthened, and the magnesium sulfate mother liquor obtained by the secondary crystallization cannot be infinitely circulated and needs to be periodically discharged.
Disclosure of Invention
Aiming at the problem that the quality of magnesium sulfate products is reduced due to impurity enrichment as the cycle number of the magnesium sulfate mother liquor is increased, the invention provides a method for preparing magnesium sulfate by using anthraquinone waste acid.
The technical scheme of the invention is as follows: a method for preparing magnesium sulfate by using anthraquinone waste acid comprises the following steps:
standing and separating the anthraquinone waste acid to obtain a dilute sulfuric acid solution and sediments;
mixing and reacting dilute sulfuric acid solution, magnesium oxide and 98 wt% 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;
heating and concentrating, cooling and crystallizing the magnesium sulfate mother liquor, and performing centrifugal separation to obtain mother liquor 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.
And further limiting, carrying out solid-liquid separation on the sediments through a vacuum rotary drum suction filter, wherein the filtrate returns to the stage of mixing and reacting the dilute sulfuric acid solution, the magnesium oxide and 98 wt% concentrated sulfuric acid, and delivering filter residues.
Further limited, the adding amount of the organic extracting agent is less than 5 percent of the mass of the mother liquor to be purified.
Further, the magnesium sulfate crystals are added in the heating concentration stage, and when the Baume degree of the magnesium sulfate mother liquor is more than or equal to 41, the heating is stopped.
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, in the cooling crystallization stage, the magnesium sulfate mother liquor after heating and concentration is cooled by adopting a water-proof cooling mode.
Further defined, in the heating concentration stage, the magnesium sulfate crystals are melted by adding superheated steam.
Further defined, the temperature of the magnesium sulfate mother liquor in the heating concentration stage is 70-80 ℃. The invention has the beneficial effects that:
1. according to the invention, the organic extractant is added, the impurity in the mother liquor to be purified is adsorbed, the mass is increased, and the sludge sediment is formed through sedimentation and accumulation, so that the purpose of layering is achieved, the sludge sediment can be removed through filtration, the purified mother liquor is returned for continuous utilization, the problems of discharge and treatment due to the fact that the magnesium sulfate solution cannot be recycled due to the enrichment of organic impurities are solved, the purity requirement of the raw material magnesium oxide is lowered, the recovery rate of magnesium sulfate is improved, and the environmental pollution is reduced.
2. According to the invention, the vacuum rotary drum suction filter is adopted to filter the sediments, the process can be continuously carried out, less manpower is required, and the filtrate in the filter residues can be recycled, so that the treatment efficiency is high and the labor cost is saved.
Drawings
FIG. 1 is a flow chart of example 1.
Detailed Description
Example 1
In this example, the concentration of the dilute sulfuric acid solution was 50 wt%.
As shown in fig. 1, a method for preparing magnesium sulfate by using anthraquinone waste acid comprises the following steps:
s1, introducing the anthraquinone waste acid into a physical sedimentation tank, standing and separating to obtain a dilute sulfuric acid solution and sediments, wherein the physical sedimentation tank has two physical sedimentation tanks in total and one physical sedimentation tank is used for standby;
s2, performing solid-liquid separation on the sediments through a vacuum drum suction filter, wherein the filtrate returns to the dilute sulfuric acid solution, and the filter cake is sent out;
s3, mixing and reacting dilute sulfuric acid solution, magnesium oxide and 98 wt% 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 delivering the filter cake;
s4, heating the magnesium sulfate mother liquor by superheated steam, adding magnesium sulfate crystals to form a saturated magnesium sulfate 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 the concentration is finished, putting 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 the Baume degree is 31 for solid-liquid separation to obtain mother liquor to be purified and magnesium sulfate crystals, and drying the magnesium sulfate crystals;
s6, adding an organic extracting agent into the mother liquor to be purified to adsorb organic impurities, increasing the mass of the organic impurities, depositing and accumulating the organic impurities to form sludge sediment, separating the sludge sediment from the liquid phase to obtain purified mother liquor and sludge sediment, mixing the purified mother liquor and the purified mother liquor, and returning to the step S4.
Example 2
In this example, the concentration of the dilute sulfuric acid solution was 40 wt%.
A method for preparing magnesium sulfate by using anthraquinone waste acid comprises the following steps:
s1, introducing the anthraquinone waste acid into a physical sedimentation tank, standing and separating to obtain a dilute sulfuric acid solution and sediments, wherein the physical sedimentation tank has two physical sedimentation tanks in total and one physical sedimentation tank is used for standby;
s2, performing solid-liquid separation on the sediments through a vacuum drum suction filter, wherein the filtrate returns to the dilute sulfuric acid solution, and the filter cake is sent out;
s3, mixing and reacting dilute sulfuric acid solution, magnesium oxide and 98 wt% 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 delivering the filter cake; s4, heating the magnesium sulfate mother liquor by superheated steam, adding magnesium sulfate crystals to form a saturated magnesium sulfate solution, wherein the temperature of the magnesium sulfate mother liquor during concentration is 80 ℃, and heating is stopped when the Baume degree of the magnesium sulfate mother liquor is 45;
s5, after the concentration is finished, putting 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 the Baume degree is 20, carrying out solid-liquid separation to obtain mother liquor to be purified and magnesium sulfate crystals, and drying the magnesium sulfate crystals;
s6, adding an organic extracting agent into the mother liquor to be purified to adsorb organic impurities, increasing the mass of the organic impurities, depositing and accumulating the organic impurities to form sludge sediment, separating the sludge sediment from the liquid phase to obtain purified mother liquor and sludge sediment, mixing the purified mother liquor and the purified mother liquor, and returning to the step S4.
Example 3
In this example, the concentration of the dilute sulfuric acid solution was 40 wt%.
A method for preparing magnesium sulfate by using anthraquinone waste acid comprises the following steps:
s1, introducing the anthraquinone waste acid into a physical sedimentation tank, standing and separating to obtain a dilute sulfuric acid solution and sediments, wherein the physical sedimentation tank has two physical sedimentation tanks in total and one physical sedimentation tank is used for standby;
s2, performing solid-liquid separation on the sediments through a vacuum drum suction filter, wherein the filtrate returns to the dilute sulfuric acid solution, and the filter cake is sent out;
s3, mixing and reacting dilute sulfuric acid solution, magnesium oxide and 98 wt% 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 delivering the filter cake;
s4, heating the magnesium sulfate mother liquor by superheated steam, adding magnesium sulfate crystals to form a saturated magnesium sulfate 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 the concentration is finished, putting the magnesium sulfate mother liquor into a flowing water bath for cooling, stopping cooling for solid-liquid separation when the temperature of the magnesium sulfate mother liquor is reduced to 25 ℃ and the Baume degree is 15 to obtain mother liquor to be purified and magnesium sulfate crystals, and drying the magnesium sulfate crystals;
s6, adding an organic extracting agent into the mother liquor to be purified to adsorb organic impurities, increasing the mass of the organic impurities, depositing and accumulating the organic impurities to form sludge sediment, separating the sludge sediment from the liquid phase to obtain purified mother liquor and sludge sediment, mixing the purified mother liquor and the purified mother liquor, and returning to the step S4.
On one hand, the discharge of magnesium sulfate mother liquor is reduced; on the other hand, the selective range of the magnesium oxide raw material is widened, the magnesium oxide with more impurities can be treated by increasing the amount of the added extracting agent, the magnesium oxide with high impurity content and the magnesium oxide with low impurity content can be mixed and put into use, and the selection is adopted by controlling reasonable ore proportioning of effective components.
From the examples 1-3, the method for preparing magnesium sulfate by using anthraquinone waste acid disclosed by the invention has the advantages that the process is simple, the impurities can be settled only by adding the organic extracting agent, the cyclic utilization of the mother liquor is realized, the utilization rate of the waste acid is improved, and the economic maximization is realized.
The method for preparing magnesium sulfate by using anthraquinone waste acid disclosed by the invention can be used for treating magnesium oxide with low 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 above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The method for preparing magnesium sulfate by using anthraquinone waste acid is characterized by comprising the following steps of:
standing and separating the anthraquinone waste acid to obtain a dilute sulfuric acid solution and sediments;
mixing and reacting dilute sulfuric acid solution, magnesium oxide and 98 wt% 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;
sequentially heating and concentrating, cooling and crystallizing the magnesium sulfate mother liquor and carrying out centrifugal separation to obtain mother liquor 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;
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 using anthraquinone waste acid according to claim 1, wherein the solid-liquid separation of the sediment is carried out by a vacuum drum filter, wherein the filtrate is returned to the mixed reaction stage of the dilute sulfuric acid solution, magnesium oxide and 98 wt% concentrated sulfuric acid, and the filter residue is sent out.
3. The method for preparing magnesium sulfate by using anthraquinone waste acid according to claim 1, wherein the addition amount of the organic extractant is less than 5% of the mass of the mother liquor to be purified.
4. 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 when the Baume degree of the magnesium sulfate mother liquor is more than or equal to 41, the heating is stopped.
5. The method for preparing magnesium sulfate by using anthraquinone waste acid according to claim 1, wherein the baume degree of magnesium sulfate mother liquor at the end of said cooling crystallization stage is less than or equal to 31.
6. The method for preparing magnesium sulfate by using anthraquinone waste acid according to claim 1, wherein in the cooling crystallization stage, the magnesium sulfate mother liquor after heating and concentration is cooled by a water-proof cooling mode.
7. The method for preparing magnesium sulfate by using anthraquinone waste acid according to claim 4, wherein in the heating concentration stage, the magnesium sulfate crystals are melted by adding superheated steam.
8. The method for preparing magnesium sulfate by using anthraquinone waste acid according to claim 7, wherein the temperature of the magnesium sulfate mother liquor in the heating concentration stage is 70-80 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116177576A (en) * | 2022-12-01 | 2023-05-30 | 百色实华环保科技有限公司 | Comprehensive utilization method of waste acid of anthraquinone production device |
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| CN116177576A (en) * | 2022-12-01 | 2023-05-30 | 百色实华环保科技有限公司 | Comprehensive utilization method of waste acid of anthraquinone production device |
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