CN112573847A - Method for removing organic matters in gypsum - Google Patents
Method for removing organic matters in gypsum Download PDFInfo
- Publication number
- CN112573847A CN112573847A CN202110073065.9A CN202110073065A CN112573847A CN 112573847 A CN112573847 A CN 112573847A CN 202110073065 A CN202110073065 A CN 202110073065A CN 112573847 A CN112573847 A CN 112573847A
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- CN
- China
- Prior art keywords
- phosphogypsum
- organic matters
- removing organic
- liquid mixture
- hydrogen peroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000010440 gypsum Substances 0.000 title claims abstract description 13
- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 13
- 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 41
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 10
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 9
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 9
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 9
- 239000005416 organic matter Substances 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 238000007790 scraping Methods 0.000 claims abstract description 5
- 230000035484 reaction time Effects 0.000 claims abstract description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract 5
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract 5
- 239000011574 phosphorus Substances 0.000 claims abstract 5
- 238000005188 flotation Methods 0.000 claims description 10
- 230000000694 effects Effects 0.000 abstract description 2
- 239000003814 drug Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- XLLIQLLCWZCATF-UHFFFAOYSA-N ethylene glycol monomethyl ether acetate Natural products COCCOC(C)=O XLLIQLLCWZCATF-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- CQRFEDVNTJTKFU-UHFFFAOYSA-N 3-methoxypentane Chemical compound CCC(CC)OC CQRFEDVNTJTKFU-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229940095564 anhydrous calcium sulfate Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/26—Calcium sulfate cements strating from chemical gypsum; starting from phosphogypsum or from waste, e.g. purification products of smoke
- C04B11/266—Chemical gypsum
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a method for removing organic matters in phosphorus gypsum, which comprises the following steps: (1) adding washing water into the phosphogypsum, standing for layering after uniformly stirring, and scraping a black organic matter layer floating on the water surface; (2) adjusting the pH value of the phosphogypsum solid-liquid mixture to 3-5, adding ferrous sulfate and hydrogen peroxide, and reacting for 1-2 hours under the stirring condition; (3) and (4) carrying out suction filtration on the phosphogypsum solid-liquid mixture to obtain the phosphogypsum with organic matters removed. The method of the invention has the advantages of simplicity, short reaction time, obvious effect and low cost.
Description
Technical Field
The invention relates to the field of impurity removal of phosphogypsum, in particular to a method for removing organic matters in the phosphogypsum.
Background
The organic matters in the phosphogypsum are mainly carried by phosphate ores and flocculating agents added during the production of phosphoric acid, and the main components of the organic matters are ethylene glycol monomethyl ether acetate, isothiocyanic methane, 3-methoxy-n-pentane, 2-ethyl-13-dioxolane and the like. The organic matter increases the standard consistency of the phosphogypsum, prolongs the setting time, reduces the strength and prevents the application of the phosphogypsum in the building material aspect.
At present, the organic matters in the dephosphorization gypsum are mainly subjected to a water washing method, a flotation method and a calcination method. The water washing method can remove most impurities and organic matters, but the sewage generated by washing must be treated for discharge or utilization. The flotation method is that water and phosphogypsum are put into flotation equipment according to a certain proportion, and organic matters floating on the water surface are separated and removed after stirring and standing. The calcining method needs to eliminate the influence of organic matters at a high temperature of 800 ℃, has high requirements on equipment, and the product is anhydrous calcium sulfate.
The flotation method can effectively remove the organic matters in the phosphogypsum only by adding a medicament, the flotation medicament is generally expensive, only a part of the organic matters can be removed without adding the medicament, and the production requirement of high-strength gypsum cannot be met.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for removing organic matters in gypsum by adopting a flotation method and a Fenton method, wherein the flotation method is used for removing the organic matters in the gypsum, and does not add a medicament and only uses a small amount of water for flotation; the Fenton method refers to Fe under acidic condition2+Catalysis H2O2The oxidative hydroxyl free radicals are generated, and a method for rapidly and nonselectively oxidizing a plurality of known organic compounds such as carboxylic acid, alcohol and ester into an inorganic state can be realized.
The technical scheme of the invention is as follows: a method for removing organic matters in phosphogypsum comprises the following steps:
(1) adding washing water into the phosphogypsum, standing for layering after uniformly stirring, and scraping a black organic matter layer floating on the water surface.
(2) Adjusting the pH value of the phosphogypsum solid-liquid mixture to 3-5, adding ferrous sulfate and hydrogen peroxide, and reacting for 1-2 hours under the stirring condition.
(3) And (4) carrying out suction filtration on the phosphogypsum solid-liquid mixture to obtain the phosphogypsum with organic matters removed.
In the step (1), the mass ratio of the washing water to the phosphogypsum is 1: 1.
In the step (2), the pH value of the phosphogypsum solid-liquid mixture is 3.5.
In the step (2), the hydrogen peroxide and the ferrous sulfate are in industrial grade, and the purity is 80%.
In the step (2), the adding amount of hydrogen peroxide is 1.5 times of the mass of the organic matters in the phosphogypsum after the flotation treatment.
In the step (2), the adding amount of the ferrous sulfate is 0.5 time of the mass of the hydrogen peroxide.
In the step (2), the reaction time was 1 hour.
In the step (3), the suction filtration pressure is 0.08 MPa.
The invention has the beneficial effects that: after the treatment by the technical scheme, the removal rate of the phosphogypsum organic matter is more than 95%. The pH value of the phosphogypsum is 3.5 after the phosphogypsum is mixed with water, and the pH value needs to be adjusted without adding a medicament. The invention has low requirement on equipment, simple process, low cost and obvious effect.
Detailed Description
Example 1
Weighing 500g of phosphogypsum in a 2000ml beaker, sampling and analyzing 0.102% of organic matters in the phosphogypsum, adding 500g of washing water, stirring uniformly, standing for 5 minutes for layering, and scraping off a black organic matter layer floating on the water surface. And measuring the pH value of the phosphogypsum solid-liquid mixture to be 3.5, adding 0.23g of ferrous sulfate and 0.45g of hydrogen peroxide, and stirring for reacting for 1 hour. And (3) carrying out suction filtration on the solid-liquid mixture after the reaction under the vacuum degree of 0.08MPa to obtain the phosphogypsum with organic matters removed, and analyzing the content of the organic matters in the phosphogypsum to be 0.005%.
Example 2
Weighing 500g of phosphogypsum in a 2000ml beaker, sampling and analyzing 0.115% of organic matters in the phosphogypsum, adding 500g of washing water, stirring uniformly, standing for 5 minutes for layering, and scraping off a black organic matter layer floating on the water surface. And measuring the pH value of the phosphogypsum solid-liquid mixture to be 3.3, adding 0.24g of ferrous sulfate and 0.48g of hydrogen peroxide, and stirring for reacting for 2 hours. And (3) carrying out suction filtration on the solid-liquid mixture after the reaction under the vacuum degree of 0.08MPa to obtain the phosphogypsum with organic matters removed, and analyzing the content of the organic matters in the phosphogypsum to be 0.007%.
Claims (8)
1. A method for removing organic matters in phosphogypsum is characterized by comprising the following steps:
(1) adding washing water into the phosphogypsum, standing for layering after uniformly stirring, and scraping a black organic matter layer floating on the water surface;
(2) adjusting the pH value of the phosphogypsum solid-liquid mixture to 3-5, adding ferrous sulfate and hydrogen peroxide, and reacting for 1-2 hours under the stirring condition;
(3) and (4) carrying out suction filtration on the phosphogypsum solid-liquid mixture to obtain the phosphogypsum with organic matters removed.
2. The method for removing organic matters in phosphorus gypsum according to claim 1, wherein in the step (1), the mass ratio of the washing water to the phosphogypsum is 1: 1.
3. The method for removing organic matters in phosphorus gypsum according to claim 1, wherein in step (2), the pH value of the phosphogypsum solid-liquid mixture is 3.5.
4. The method for removing organic matters in phosphorus gypsum according to claim 1, wherein in the step (2), the hydrogen peroxide and the ferrous sulfate are of industrial grade, and the purity of each is 80%.
5. The method for removing organic matters in phosphogypsum according to claim 1, wherein in the step (2), the adding amount of hydrogen peroxide is 1.5 times of the mass of the organic matters in the phosphogypsum after flotation treatment.
6. The method for removing organic matters in phosphorus gypsum according to claim 1, wherein in the step (2), the addition amount of the ferrous sulfate is 0.5 times of the mass of the hydrogen peroxide.
7. The method for removing organic matters in gypsum according to claim 1, wherein the reaction time in step (2) is 1 hour.
8. The method for removing organic matters in gypsum according to claim 1, wherein in the step (3), the suction filtration pressure is 0.08 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110073065.9A CN112573847A (en) | 2021-01-20 | 2021-01-20 | Method for removing organic matters in gypsum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110073065.9A CN112573847A (en) | 2021-01-20 | 2021-01-20 | Method for removing organic matters in gypsum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112573847A true CN112573847A (en) | 2021-03-30 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110073065.9A Pending CN112573847A (en) | 2021-01-20 | 2021-01-20 | Method for removing organic matters in gypsum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112573847A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113135585A (en) * | 2021-04-22 | 2021-07-20 | 深圳市青青源科技有限公司 | Preparation method for reducing organic matter content in desulfurized gypsum |
| CN115893885A (en) * | 2022-12-02 | 2023-04-04 | 湖北省生态环保有限公司 | Phosphogypsum immersion cleaning agent and phosphogypsum harmless treatment method |
| CN116573661A (en) * | 2023-06-08 | 2023-08-11 | 西南科技大学 | A method for removing organic matter with phosphogypsum |
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| CN104556188A (en) * | 2013-10-14 | 2015-04-29 | 青岛市首胜实业有限公司 | Washing and purifying method of phosphogypsum |
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| CN106006698A (en) * | 2016-05-23 | 2016-10-12 | 中国建筑第八工程局有限公司 | Phosphorus gypsum purification treatment method |
| CN108467016A (en) * | 2018-06-11 | 2018-08-31 | 华东理工大学 | A method of fluorine element being extracted from industrial gypsum using flotation technology |
| CN109987750A (en) * | 2019-04-28 | 2019-07-09 | 南京大学 | A method for promoting Fenton oxidation mediated by calcium and organic acid complexes |
| CN109987749A (en) * | 2019-04-28 | 2019-07-09 | 南京大学 | A Control Method for Promoting Fenton Oxidation Mediated by Calcium and Organic Acid Complexes |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113135585A (en) * | 2021-04-22 | 2021-07-20 | 深圳市青青源科技有限公司 | Preparation method for reducing organic matter content in desulfurized gypsum |
| CN115893885A (en) * | 2022-12-02 | 2023-04-04 | 湖北省生态环保有限公司 | Phosphogypsum immersion cleaning agent and phosphogypsum harmless treatment method |
| CN116573661A (en) * | 2023-06-08 | 2023-08-11 | 西南科技大学 | A method for removing organic matter with phosphogypsum |
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Application publication date: 20210330 |