CN111792663A - Ardealite whitening method - Google Patents
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- CN111792663A CN111792663A CN202010679570.3A CN202010679570A CN111792663A CN 111792663 A CN111792663 A CN 111792663A CN 202010679570 A CN202010679570 A CN 202010679570A CN 111792663 A CN111792663 A CN 111792663A
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- phosphogypsum
- calcining
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- 230000002087 whitening effect Effects 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 27
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims abstract description 67
- 238000001354 calcination Methods 0.000 claims abstract description 64
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 32
- 238000005406 washing Methods 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 10
- 238000002386 leaching Methods 0.000 claims abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 239000000463 material Substances 0.000 claims description 28
- 239000000725 suspension Substances 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 239000000706 filtrate Substances 0.000 claims description 11
- 230000007935 neutral effect Effects 0.000 claims description 9
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 7
- 239000001099 ammonium carbonate Substances 0.000 claims description 7
- 239000012295 chemical reaction liquid Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 4
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 3
- 239000005695 Ammonium acetate Substances 0.000 claims description 3
- 239000004254 Ammonium phosphate Substances 0.000 claims description 3
- 229940043376 ammonium acetate Drugs 0.000 claims description 3
- 235000019257 ammonium acetate Nutrition 0.000 claims description 3
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 3
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 3
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 3
- RYYXDZDBXNUPOG-UHFFFAOYSA-N 4,5,6,7-tetrahydro-1,3-benzothiazole-2,6-diamine;dihydrochloride Chemical compound Cl.Cl.C1C(N)CCC2=C1SC(N)=N2 RYYXDZDBXNUPOG-UHFFFAOYSA-N 0.000 claims description 2
- LXAHHHIGZXPRKQ-UHFFFAOYSA-N 5-fluoro-2-methylpyridine Chemical compound CC1=CC=C(F)C=N1 LXAHHHIGZXPRKQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000002639 sodium chloride Nutrition 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 10
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 3
- 150000004706 metal oxides Chemical class 0.000 abstract description 3
- 238000005554 pickling Methods 0.000 abstract description 3
- 239000010440 gypsum Substances 0.000 description 8
- 229910052602 gypsum Inorganic materials 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical compound [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002367 phosphate rock Substances 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/468—Purification of calcium sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a phosphogypsum whitening method, which comprises the steps of calcining, acid leaching and washing, wherein phosphogypsum is used as a raw material, the whiteness of the phosphogypsum of about 20 percent of the raw material can be improved to be more than 90 by utilizing the method, the whiteness of the phosphogypsum is greatly improved, the problem that the application of the phosphogypsum is limited in some aspects due to low whiteness can be solved, and the additional value of the phosphogypsum is further improved; the calcining auxiliary agent can react with metal impurities to generate a compound which can be removed by washing and pickling, and the defect that the whiteness of the phosphogypsum is not remarkably improved due to the fact that insoluble metal oxides are generated by direct calcining is overcome.
Description
Technical Field
The invention relates to a phosphogypsum whitening method.
Background
Phosphogypsum is a solid waste discharged in the production of wet-process phosphoric acid. At present, the accumulated stacking quantity of phosphogypsum in China exceeds 2.5 hundred million tons, and the annual emission quantity reaches 7000 million tons. Because the phosphogypsum has high impurity content and complex components, such as undecomposed phosphorite, phosphoric acid, calcium fluoride, iron, aluminum compounds, organic matters and other impurities, the whiteness of the phosphogypsum is low, and the phosphogypsum is generally light yellow, light grey or grey black, the phosphogypsum can only be used for cement industry, chemical raw materials, soil conditioners, roadbeds or industrial fillers and the like, and although the utilization ways of the phosphogypsum are more, the resource utilization rate is always low and the added value is not high. If the phosphogypsum is subjected to impurity removal and purification to prepare the white gypsum, the utilization value of the phosphogypsum can be greatly improved, the natural white gypsum with high price and scarcity can be replaced, and the consumption of mineral resources and the damage to the ecology are reduced.
Patent CN102923752A describes a technical method for whitening phosphogypsum, but the method has no effect and is not significant for gypsum with lower whiteness, and the whiteness of the whitened gypsum is not significantly improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention solves the problems that: provides a phosphogypsum whitening method with good whitening effect.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a method for whitening phosphogypsum, which comprises the following steps:
s1, calcining: placing the phosphogypsum and the calcining auxiliary agent into a heating container for calcining, and taking out for later use after cooling to obtain a calcined material; the calcination auxiliary agent is one of ammonium acetate, ammonium carbonate, ammonium phosphate, ammonium bicarbonate, sodium chloride, EDTA disodium and thiourea dioxide;
s2, acid leaching: drying the calcined material calcined in the step S1, and mixing the dried calcined material with water to form a suspension; putting the suspension into a reaction vessel, adding a sulfuric acid solution into the reaction vessel, putting the reaction vessel into a constant-temperature water bath kettle, and stirring for reaction;
s3, washing: and (5) after the reaction in the step S2 is finished, cooling the reaction liquid, performing suction filtration, washing until the filtrate is neutral, drying, and whitening.
Further, the mass ratio of the phosphogypsum to the calcining auxiliary agent in the step S1 is 0.0005-0.06: 1.
further, in the step S1, the calcining temperature of the phosphogypsum and the calcining auxiliary agent is 500-700 ℃; the calcination time is 1-3 h.
Further, in the step S2, the mass ratio of the calcined material to the water is 1: 4-8.
Further, in the step S2, the mass ratio of the suspension to the sulfuric acid solution is 1: 8-1: 20; the concentration of the sulfuric acid solution is 1-2 mol/L.
Further, in the step S2, the temperature in the constant temperature water bath is 50 to 100 ℃.
Further, in the step S3, the filtrate is washed until the filtrate is neutral, and then dried at 45 ℃.
The invention has the advantages of
The invention provides a phosphogypsum whitening method, which takes phosphogypsum as a raw material, can improve the whiteness of the phosphogypsum to more than 90 by using the method, greatly improves the whiteness of the phosphogypsum, can solve the problem that the application of the phosphogypsum is limited in some aspects due to low whiteness, and further improves the additional value of the phosphogypsum; the calcining auxiliary agent can react with metal impurities to generate a compound which can be removed by washing and pickling, and the defect that the whiteness of the phosphogypsum is not remarkably improved due to the fact that insoluble metal oxides are generated by direct calcining is overcome.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1
As shown in fig. 1, a method for whitening phosphogypsum comprises the following steps:
s1, calcining: placing the phosphogypsum and the calcining auxiliary agent into a heating container for calcining, and taking out for later use after cooling to obtain a calcined material; the calcination auxiliary agent is ammonium bicarbonate; the mass ratio of the phosphogypsum to the calcining auxiliary agent is 0.0005: 1; the calcining temperature of the phosphogypsum and the calcining auxiliary agent is 600 ℃; the calcination time was 2 h.
S2, acid leaching: drying the calcined material calcined in the step S1, and mixing the dried calcined material with water to form a suspension; the mass ratio of the calcined material to the water is 1: 4; putting the suspension into a reaction vessel, adding a sulfuric acid solution into the reaction vessel, putting the reaction vessel into a constant-temperature water bath kettle, and stirring for reaction; the mass ratio of the suspension to the sulfuric acid solution is 1: 8; the concentration of the sulfuric acid solution is 1 mol/L; the temperature in the constant temperature water bath was 50 ℃.
S3, washing: and (5) after the reaction in the step S2 is finished, cooling the reaction liquid, performing suction filtration, washing until the filtrate is neutral, drying at 45 ℃, and finishing whitening. The whiteness was measured to be 92.0.
Example 2
As shown in fig. 1, a method for whitening phosphogypsum comprises the following steps:
s1, calcining: placing the phosphogypsum and the calcining auxiliary agent into a heating container for calcining, and taking out for later use after cooling to obtain a calcined material; the calcination auxiliary agent is ammonium phosphate; the mass ratio of the phosphogypsum to the calcining auxiliary agent is 0.0008: 1; the calcining temperature of the phosphogypsum and the calcining auxiliary agent is 700 ℃; the calcination time was 2 h.
S2, acid leaching: drying the calcined material calcined in the step S1, and mixing the dried calcined material with water to form a suspension; the mass ratio of the calcined material to the water is 1: 8; putting the suspension into a reaction vessel, adding a sulfuric acid solution into the reaction vessel, putting the reaction vessel into a constant-temperature water bath kettle, and stirring for reaction; the mass ratio of the suspension to the sulfuric acid solution is 1: 10; the concentration of the sulfuric acid solution is 2 mol/L; the temperature in the constant temperature water bath was 60 ℃.
S3, washing: and (5) after the reaction in the step S2 is finished, cooling the reaction liquid, performing suction filtration, washing until the filtrate is neutral, drying at 45 ℃, and finishing whitening. The whiteness was measured to be 92.5.
Example 3
As shown in fig. 1, a method for whitening phosphogypsum comprises the following steps:
s1, calcining: placing the phosphogypsum and the calcining auxiliary agent into a heating container for calcining, and taking out for later use after cooling to obtain a calcined material; the calcining auxiliary agent is ammonium carbonate; the mass ratio of the phosphogypsum to the calcining auxiliary agent is 0.001: 1; the calcining temperature of the phosphogypsum and the calcining auxiliary agent is 500 ℃; the calcination time was 2 h.
S2, acid leaching: drying the calcined material calcined in the step S1, and mixing the dried calcined material with water to form a suspension; the mass ratio of the calcined material to the water is 1: 6; putting the suspension into a reaction vessel, adding a sulfuric acid solution into the reaction vessel, putting the reaction vessel into a constant-temperature water bath kettle, and stirring for reaction; the mass ratio of the suspension to the sulfuric acid solution is 1: 14; the concentration of the sulfuric acid solution is 1.5 mol/L; the temperature in the constant temperature water bath was 70 ℃.
S3, washing: and (5) after the reaction in the step S2 is finished, cooling the reaction liquid, performing suction filtration, washing until the filtrate is neutral, drying at 45 ℃, and finishing whitening. The whiteness was measured to be 91.8.
Example 4
As shown in fig. 1, a method for whitening phosphogypsum comprises the following steps:
s1, calcining: placing the phosphogypsum and the calcining auxiliary agent into a heating container for calcining, and taking out for later use after cooling to obtain a calcined material; the calcination auxiliary agent is ammonium acetate; the mass ratio of the phosphogypsum to the calcining auxiliary agent is 0.03: 1; the calcining temperature of the phosphogypsum and the calcining auxiliary agent is 700 ℃; the calcination time was 3 h.
S2, acid leaching: drying the calcined material calcined in the step S1, and mixing the dried calcined material with water to form a suspension; the mass ratio of the calcined material to the water is 1: 6; putting the suspension into a reaction vessel, adding a sulfuric acid solution into the reaction vessel, putting the reaction vessel into a constant-temperature water bath kettle, and stirring for reaction; the mass ratio of the suspension to the sulfuric acid solution is 1: 16; the concentration of the sulfuric acid solution is 1 mol/L; the temperature in the constant temperature water bath was 85 ℃.
S3, washing: and (5) after the reaction in the step S2 is finished, cooling the reaction liquid, performing suction filtration, washing until the filtrate is neutral, drying at 45 ℃, and finishing whitening. The whiteness was measured to be 91.5.
Example 5
As shown in fig. 1, a method for whitening phosphogypsum comprises the following steps:
s1, calcining: placing the phosphogypsum and the calcining auxiliary agent into a heating container for calcining, and taking out for later use after cooling to obtain a calcined material; the calcination auxiliary agent is ammonium bicarbonate; the mass ratio of the phosphogypsum to the calcining auxiliary agent is 0.06: 1; the calcining temperature of the phosphogypsum and the calcining auxiliary agent is 600 ℃; the calcination time is 1 h.
S2, acid leaching: drying the calcined material calcined in the step S1, and mixing the dried calcined material with water to form a suspension; the mass ratio of the calcined material to the water is 1: 5; putting the suspension into a reaction vessel, adding a sulfuric acid solution into the reaction vessel, putting the reaction vessel into a constant-temperature water bath kettle, and stirring for reaction; the mass ratio of the suspension to the sulfuric acid solution is 1: 20; the concentration of the sulfuric acid solution is 1 mol/L; the temperature in the constant temperature water bath kettle is 100 ℃.
S3, washing: and (5) after the reaction in the step S2 is finished, cooling the reaction liquid, performing suction filtration, washing until the filtrate is neutral, drying at 45 ℃, and finishing whitening. The whiteness was measured to be 92.8.
The gypsum contains metal impurities such as iron and the like, impurities such as indissolvable iron oxide and the like are generated by high-temperature calcination, acid leaching cannot be well removed, the whiteness of the gypsum is obviously reduced, the calcination auxiliary agent can react with the metal impurities such as iron and the like in the gypsum, the indissolvable iron oxide salt with dark color is avoided, and (NH) can be generated through an ammonium compound4)3Fe（PO4）2The colorless and easily soluble impurities can be directly removed by water washing or acid washing, and the whiteness of the gypsum is obviously improved. The invention provides a phosphogypsum whitening method, which takes phosphogypsum as a raw material, can improve the whiteness of the phosphogypsum to more than 90 by using the method, greatly improves the whiteness of the phosphogypsum, can solve the problem that the application of the phosphogypsum is limited in some aspects due to low whiteness, and further improves the additional value of the phosphogypsum; the calcining auxiliary agent can react with metal impurities to generate a compound which can be removed by washing and pickling, and the defect that the whiteness of the phosphogypsum is not remarkably improved due to the fact that insoluble metal oxides are generated by direct calcining is overcome.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. The phosphogypsum whitening method is characterized by comprising the following steps:
s1, calcining: placing the phosphogypsum and the calcining auxiliary agent into a heating container for calcining, and taking out for later use after cooling to obtain a calcined material; the calcination auxiliary agent is one of ammonium acetate, ammonium carbonate, ammonium phosphate, ammonium bicarbonate, sodium chloride, EDTA disodium and thiourea dioxide;
s2, acid leaching: drying the calcined material calcined in the step S1, and mixing the dried calcined material with water to form a suspension; putting the suspension into a reaction vessel, adding a sulfuric acid solution into the reaction vessel, putting the reaction vessel into a constant-temperature water bath kettle, and stirring for reaction;
s3, washing: and (5) after the reaction in the step S2 is finished, cooling the reaction liquid, performing suction filtration, washing until the filtrate is neutral, drying, and whitening.
2. The phosphogypsum whitening method according to claim 1, characterized in that the mass ratio of the phosphogypsum to the calcining auxiliary agent in the step S1 is 0.0005-0.06: 1.
3. the phosphogypsum whitening method according to claim 1, characterized in that in the step S1, the calcining temperature of the phosphogypsum and the calcining auxiliary agent is 500-700 ℃; the calcination time is 1-3 h.
4. The phosphogypsum whitening method according to claim 1, characterized in that in the step S2, the mass ratio of the calcined material to the water is 1: 4-8.
5. The phosphogypsum whitening method according to claim 1, characterized in that in the step S2, the mass ratio of the suspension to the sulfuric acid solution is 1: 8-1: 20; the concentration of the sulfuric acid solution is 1-2 mol/L.
6. The phosphogypsum whitening method according to claim 1, characterized in that in the step S2, the temperature in the constant temperature water bath is 50-100 ℃.
7. The phosphogypsum whitening method according to claim 1, characterized in that in the step S3, the filtrate is washed until the filtrate is neutral and then dried at 45 ℃.
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| CN202010679570.3A CN111792663A (en) | 2020-07-15 | 2020-07-15 | Ardealite whitening method |
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Cited By (4)
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| CN113072046A (en) * | 2021-04-09 | 2021-07-06 | 郑州大学 | Method for removing impurities and improving whiteness of phosphogypsum through flotation method |
| CN113620625A (en) * | 2021-09-15 | 2021-11-09 | 江苏一夫科技股份有限公司 | Method for removing impurities from phosphogypsum and preparing white anhydrous phosphogypsum |
| CN114477815A (en) * | 2022-03-03 | 2022-05-13 | 云南云天化股份有限公司 | Method for quickly whitening phosphogypsum |
| CN116425187A (en) * | 2023-04-20 | 2023-07-14 | 湖南科技大学 | A method for improving the whiteness of phosphogypsum |
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| CN113620625A (en) * | 2021-09-15 | 2021-11-09 | 江苏一夫科技股份有限公司 | Method for removing impurities from phosphogypsum and preparing white anhydrous phosphogypsum |
| CN114477815A (en) * | 2022-03-03 | 2022-05-13 | 云南云天化股份有限公司 | Method for quickly whitening phosphogypsum |
| CN114477815B (en) * | 2022-03-03 | 2023-01-31 | 云南云天化股份有限公司 | Method for rapidly whitening phosphogypsum |
| CN116425187A (en) * | 2023-04-20 | 2023-07-14 | 湖南科技大学 | A method for improving the whiteness of phosphogypsum |
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