CN112110470A - Phosphogypsum waste residue treatment method - Google Patents
Phosphogypsum waste residue treatment method Download PDFInfo
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- CN112110470A CN112110470A CN202011019690.7A CN202011019690A CN112110470A CN 112110470 A CN112110470 A CN 112110470A CN 202011019690 A CN202011019690 A CN 202011019690A CN 112110470 A CN112110470 A CN 112110470A
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- solution
- waste residue
- phosphogypsum
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- reaction
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- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 title claims abstract description 66
- 239000002699 waste material Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 21
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000003756 stirring Methods 0.000 claims abstract description 32
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000013078 crystal Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000007787 solid Substances 0.000 claims abstract description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 13
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000007873 sieving Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 2
- 235000011187 glycerol Nutrition 0.000 description 10
- 238000004090 dissolution Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002894 chemical waste Substances 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000010440 gypsum Substances 0.000 description 2
- 229910052602 gypsum Inorganic materials 0.000 description 2
- -1 hydrogen ions Chemical class 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000000463 material Substances 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
- 239000002861 polymer material Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 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
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/468—Purification of calcium sulfates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01F11/466—Conversion of one form of calcium sulfate to another
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- 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
Abstract
The invention discloses a phosphogypsum waste residue treatment method, which comprises the following steps: washing and drying the phosphogypsum waste residue by using deionized water, and then grinding and sieving to prepare pretreated phosphogypsum powder; mixing glycerol and absolute ethyl alcohol, stirring uniformly, adding dodecyl trimethyl ammonium bromide, and continuously stirring until the solid is dissolved to prepare a solution A; mixing and stirring the prepared pre-treated phosphogypsum powder and a nitric acid solution, adding a sulfuric acid solution, continuously stirring to prepare a solution B, slowly dropwise adding the prepared solution A into the solution B, carrying out intermittent ultrasonic treatment, transferring the prepared mixture into a reaction kettle, carrying out reaction, cooling to room temperature after the reaction is finished, filtering the reaction liquid, and drying the solid obtained by filtering to prepare the nano calcium sulfate crystal. The method is simple to operate, and the prepared nano calcium sulfate crystal has good stability, the particle size of 30-50nm and good dispersion.
Description
The technical field is as follows:
the invention relates to the field of building materials, in particular to a phosphogypsum waste residue treatment method.
Background art:
the phosphogypsum is waste residue in the chemical fertilizer industry for producing phosphoric acid and ammonium phosphate by using a phosphorite powder wet method, has acidity and seriously pollutes the environment, is seen as first chemical waste residue by all countries in the world, and how to treat the waste residue becomes a very concerned problem for all countries. The outline of the 'eleven-five' planning is also provided, the comprehensive utilization of resources is well grabbed, and the utilization of industrial wastes such as fly ash, coal gangue, metallurgical and chemical waste residues and tailings is promoted. The comprehensive utilization of industrial wastes is an important part for developing the recycling economy and building a resource-saving society, and the state sets special preferential policies including tax deduction and avoidance and the like for comprehensive utilization projects.
The key is how to treat and reuse the phosphogypsum waste residue. The nanometer calcium sulfate crystal is an inorganic powder material, can be used as a reinforcement to be applied to a high polymer material, and has the advantages of good dispersion, uniform structure, large specific surface area, excellent performance and low price. At present, the raw materials for preparing the nano calcium sulfate crystal are mainly prepared by taking natural gypsum or gypsum as raw materials, and the research on preparing the nano calcium sulfate crystal by using phosphogypsum waste residues is less.
The invention content is as follows:
the invention aims to solve the technical problem of providing a phosphogypsum waste residue treatment method aiming at the defects of the prior art, the method is simple to operate, and the prepared nano calcium sulfate crystal has good stability, the particle size of 30-50nm and good dispersion.
In order to solve the technical problems, the invention adopts the following technical scheme:
a phosphogypsum waste residue treatment method comprises the following steps:
(1) washing and drying the phosphogypsum waste residue by using deionized water, and then grinding and sieving to prepare pretreated phosphogypsum powder;
(2) mixing glycerol and absolute ethyl alcohol, stirring uniformly, adding dodecyl trimethyl ammonium bromide, and continuously stirring until the solid is dissolved to prepare a solution A;
(3) mixing and stirring the prepared pre-treated phosphogypsum powder and a nitric acid solution, adding a sulfuric acid solution, continuously stirring to prepare a solution B, slowly dropwise adding the prepared solution A into the solution B, carrying out intermittent ultrasonic treatment, transferring the prepared mixture into a reaction kettle, carrying out reaction, cooling to room temperature after the reaction is finished, filtering the reaction liquid, and drying the solid obtained by filtering to prepare the nano calcium sulfate crystal.
Preferably, in the step (2), the ratio of the glycerol to the absolute ethyl alcohol to the dodecyl trimethyl ammonium bromide is (0.35-0.55) g: 60 ml: (25-35) ml.
Preferably, in the step (3), the usage ratio of the phosphogypsum waste residue to the nitric acid solution to the sulfuric acid solution is (1.5-2.5) g: 2 ml: 2 ml.
Preferably, in the step (3), the dropping rate of the solution A is 1.2 to 1.5 ml/min.
Preferably, in the step (3), the conditions of the batch-type ultrasonic treatment are as follows: performing ultrasonic treatment at power of 400-500W for 10min, stopping for 1min, and repeating the above steps for 1-3 h.
Preferably, in the step (3), the reaction conditions are as follows: the temperature is 120-150 ℃ and the time is 15-30 h.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
firstly, preprocessing phosphogypsum waste residues; and then, dissolving the pretreated phosphogypsum waste residue powder by using a nitric acid solution and reacting with a sulfuric acid solution by using a mixture of glycerol and ethanol as a solvent and dodecyl trimethyl ammonium bromide as a surfactant to prepare the nano calcium sulfate crystal. The ethanol has low boiling point and is easier to volatilize at the reaction temperature, thereby greatly improving the pressure in the reaction kettle and being beneficial to controlling the form of crystals. The phosphogypsum waste residue is an insoluble electrolyte and has low solubility in water, the phosphogypsum waste residue is dissolved by a nitric acid solution, and hydrogen ions generated by the ionization of nitric acid and sulfate ions generated by the dissolution of calcium sulfate dihydrate are combined to form bisulfate ions, so that the dissolution of the calcium sulfate dihydrate is promoted; calcium sulfate crystal nuclei are formed when the concentration of calcium ions and sulfate ions in the solution is saturated; the invention also adds glycerin which can promote the dissolution of calcium sulfate dihydrate and is added into supersaturated solution to form, and the glycerin can be selectively adsorbed on the surface of the calcium sulfate, so that the calcium sulfate grows along the C axis to finally generate the nanometer calcium sulfate. The invention also adds dodecyl trimethyl ammonium bromide as a surfactant, which can effectively control the selective growth of the calcium sulfate crystal, thereby conditioning the shape of the prepared nano calcium sulfate crystal. The average diameter of the calcium sulfate crystal prepared by the method is 30-50 nm.
The specific implementation mode is as follows:
the present invention is further illustrated by the following examples, which are provided for the purpose of illustration only and are not intended to be limiting.
Example 1
(1) Washing and drying the phosphogypsum waste residue by using deionized water, and then grinding and sieving to prepare pretreated phosphogypsum powder;
(2) mixing 60ml of glycerol and 25ml of absolute ethyl alcohol, uniformly stirring, adding 0.35g of dodecyl trimethyl ammonium bromide, and continuously stirring until the solid is dissolved to prepare a solution A;
(3) mixing and stirring 1.5g of the prepared pretreated phosphogypsum powder and 2ml of nitric acid solution, adding 2ml of sulfuric acid solution, continuously stirring to prepare solution B, slowly dropwise adding the prepared solution A into the solution B, wherein the dropwise adding speed of the solution A is 1.2ml/min, and adopting intermittent ultrasonic treatment, wherein the specific process is as follows: performing ultrasonic treatment at 400W for 10min, stopping for 1min, and repeating the above steps for 1 h; and transferring the prepared mixture into a reaction kettle, reacting for 15 hours at 120 ℃, cooling to room temperature after the reaction is finished, filtering the reaction liquid, and drying the solid obtained by filtering to obtain the nano calcium sulfate crystal.
Example 2
(1) Washing and drying the phosphogypsum waste residue by using deionized water, and then grinding and sieving to prepare pretreated phosphogypsum powder;
(2) mixing 60ml of glycerol and 35ml of absolute ethyl alcohol, uniformly stirring, adding 0.55g of dodecyl trimethyl ammonium bromide, and continuously stirring until the solid is dissolved to prepare a solution A;
(3) mixing and stirring 2.5g of the prepared pretreated phosphogypsum powder and 2ml of nitric acid solution, adding 2ml of sulfuric acid solution, continuously stirring to prepare solution B, slowly dropwise adding the prepared solution A into the solution B, wherein the dropwise adding speed of the solution A is 1.5ml/min, and adopting intermittent ultrasonic treatment, wherein the specific process is as follows: performing ultrasonic treatment at 500W for 10min, stopping for 1min, and repeating the above steps for 3 h; and transferring the prepared mixture into a reaction kettle, reacting for 30 hours at 150 ℃, cooling to room temperature after the reaction is finished, filtering the reaction liquid, and drying the solid obtained by filtering to obtain the nano calcium sulfate crystal.
Example 3
(1) Washing and drying the phosphogypsum waste residue by using deionized water, and then grinding and sieving to prepare pretreated phosphogypsum powder;
(2) mixing 60ml of glycerol and 30ml of absolute ethyl alcohol, uniformly stirring, adding 0.4g of dodecyl trimethyl ammonium bromide, and continuously stirring until the solid is dissolved to prepare a solution A;
(3) mixing and stirring 2g of the prepared pretreated phosphogypsum powder and 2ml of nitric acid solution, adding 2ml of sulfuric acid solution, continuously stirring to prepare solution B, slowly dropwise adding the prepared solution A into the solution B, wherein the dropwise adding speed of the solution A is 1.2ml/min, and performing intermittent ultrasonic treatment, wherein the specific process comprises the following steps: performing ultrasonic treatment at power of 450W for 10min, stopping for 1min, and repeating the above steps for 2 h; and transferring the prepared mixture into a reaction kettle, reacting for 20 hours at 130 ℃, cooling to room temperature after the reaction is finished, filtering the reaction liquid, and drying the solid obtained by filtering to obtain the nano calcium sulfate crystal.
Example 4
(1) Washing and drying the phosphogypsum waste residue by using deionized water, and then grinding and sieving to prepare pretreated phosphogypsum powder;
(2) mixing 60ml of glycerol and 30ml of absolute ethyl alcohol, uniformly stirring, adding 0.5g of dodecyl trimethyl ammonium bromide, and continuously stirring until the solid is dissolved to prepare a solution A;
(3) mixing and stirring 2g of the prepared pretreated phosphogypsum powder and 2ml of nitric acid solution, adding 2ml of sulfuric acid solution, continuously stirring to prepare solution B, slowly dropwise adding the prepared solution A into the solution B, wherein the dropwise adding speed of the solution A is 1.5ml/min, and performing intermittent ultrasonic treatment, wherein the specific process comprises the following steps: performing ultrasonic treatment at 400W for 10min, stopping for 1min, and repeating the above steps for 2 h; and transferring the prepared mixture into a reaction kettle, reacting for 20 hours at 130 ℃, cooling to room temperature after the reaction is finished, filtering the reaction liquid, and drying the solid obtained by filtering to obtain the nano calcium sulfate crystal.
Example 5
(1) Washing and drying the phosphogypsum waste residue by using deionized water, and then grinding and sieving to prepare pretreated phosphogypsum powder;
(2) mixing 60ml of glycerol and 30ml of absolute ethyl alcohol, uniformly stirring, adding 0.45g of dodecyl trimethyl ammonium bromide, and continuously stirring until the solid is dissolved to prepare a solution A;
(3) mixing and stirring 2g of the prepared pretreated phosphogypsum powder and 2ml of nitric acid solution, adding 2ml of sulfuric acid solution, continuously stirring to prepare solution B, slowly dropwise adding the prepared solution A into the solution B, wherein the dropwise adding speed of the solution A is 1.3ml/min, and performing intermittent ultrasonic treatment, wherein the specific process comprises the following steps: performing ultrasonic treatment at 500W for 10min, stopping for 1min, and repeating the above steps for 2 h; and transferring the prepared mixture into a reaction kettle, reacting for 30 hours at 140 ℃, cooling to room temperature after the reaction is finished, filtering the reaction liquid, and drying the solid obtained by filtering to obtain the nano calcium sulfate crystal.
Although specific embodiments of the invention have been described, many other forms and modifications of the invention will be apparent to those skilled in the art. It is to be understood that the appended claims and this invention generally cover all such obvious forms and modifications which are within the true spirit and scope of the present invention.
Claims (6)
1. The phosphogypsum waste residue treatment method is characterized by comprising the following steps:
(1) washing and drying the phosphogypsum waste residue by using deionized water, and then grinding and sieving to prepare pretreated phosphogypsum powder;
(2) mixing glycerol and absolute ethyl alcohol, stirring uniformly, adding dodecyl trimethyl ammonium bromide, and continuously stirring until the solid is dissolved to prepare a solution A;
(3) mixing and stirring the prepared pre-treated phosphogypsum powder and a nitric acid solution, adding a sulfuric acid solution, continuously stirring to prepare a solution B, slowly dropwise adding the prepared solution A into the solution B, carrying out intermittent ultrasonic treatment, transferring the prepared mixture into a reaction kettle, carrying out reaction, cooling to room temperature after the reaction is finished, filtering the reaction liquid, and drying the solid obtained by filtering to prepare the nano calcium sulfate crystal.
2. The phosphogypsum waste residue treatment method according to claim 1, which is characterized in that: in the step (2), the dosage ratio of the glycerol to the absolute ethyl alcohol to the dodecyl trimethyl ammonium bromide is (0.35-0.55) g: 60 ml: (25-35) ml.
3. The phosphogypsum waste residue treatment method according to claim 1, which is characterized in that: in the step (3), the dosage ratio of the phosphogypsum waste residue to the nitric acid solution to the sulfuric acid solution is (1.5-2.5) g: 2 ml: 2 ml.
4. The phosphogypsum waste residue treatment method according to claim 1, which is characterized in that: in the step (3), the dropping speed of the solution A is 1.2-1.5 ml/min.
5. The phosphogypsum waste residue treatment method according to claim 1, which is characterized in that: in the step (3), the conditions of the intermittent ultrasonic treatment are as follows: performing ultrasonic treatment at power of 400-500W for 10min, stopping for 1min, and repeating the above steps for 1-3 h.
6. The phosphogypsum waste residue treatment method according to claim 1, which is characterized in that: in the step (3), the reaction conditions are as follows: the temperature is 120-150 ℃ and the time is 15-30 h.
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CN202011019690.7A CN112110470A (en) | 2020-09-25 | 2020-09-25 | Phosphogypsum waste residue treatment method |
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CN202011019690.7A CN112110470A (en) | 2020-09-25 | 2020-09-25 | Phosphogypsum waste residue treatment method |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112978782A (en) * | 2021-04-16 | 2021-06-18 | 贵州大学 | Preparation method of nano flaky calcium sulfate |
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CN101844749A (en) * | 2010-02-11 | 2010-09-29 | 汪晋强 | Method for producing concentrated sulfuric acid and co-producing industrial salt and gypsum by using phosphogypsum |
CN102634843A (en) * | 2012-04-27 | 2012-08-15 | 昆明理工大学 | Method for preparing micron-sized calcium sulfate particles and crystal whiskers from phosphogypsum |
CA2852131A1 (en) * | 2011-10-24 | 2013-05-02 | Hydrometal Sa | Method for treating phosphate rock |
CN105088347A (en) * | 2015-08-04 | 2015-11-25 | 合肥学院 | Method for utilizing solid waste ardealite to prepare gypsum whiskers |
CN110342560A (en) * | 2019-07-30 | 2019-10-18 | 贵州大学 | A method of waterless nano calcium sulfate is prepared based on ardealite |
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2020
- 2020-09-25 CN CN202011019690.7A patent/CN112110470A/en active Pending
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