CN115716721A - Method for directly preparing anhydrous gypsum by using phosphogypsum - Google Patents
Method for directly preparing anhydrous gypsum by using phosphogypsum Download PDFInfo
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- CN115716721A CN115716721A CN202211479054.1A CN202211479054A CN115716721A CN 115716721 A CN115716721 A CN 115716721A CN 202211479054 A CN202211479054 A CN 202211479054A CN 115716721 A CN115716721 A CN 115716721A
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- phosphogypsum
- anhydrous gypsum
- acid solution
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- metal ions
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- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 title claims abstract description 47
- 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 44
- 238000000034 method Methods 0.000 title claims abstract description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 42
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000002253 acid Substances 0.000 claims abstract description 28
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 239000000725 suspension Substances 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 10
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 230000009466 transformation Effects 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 3
- -1 aluminum ions Chemical class 0.000 claims description 8
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims 1
- 229910001415 sodium ion Inorganic materials 0.000 claims 1
- 238000001354 calcination Methods 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000006477 desulfuration reaction Methods 0.000 abstract description 2
- 230000023556 desulfurization Effects 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000007795 chemical reaction product Substances 0.000 description 28
- 238000001914 filtration Methods 0.000 description 6
- 229910052602 gypsum Inorganic materials 0.000 description 6
- 239000010440 gypsum Substances 0.000 description 6
- 229940095564 anhydrous calcium sulfate Drugs 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910052925 anhydrite Inorganic materials 0.000 description 3
- 229940095672 calcium sulfate Drugs 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011507 gypsum plaster Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method for directly preparing anhydrous gypsum by using phosphogypsum, which comprises the steps of mixing an acid solution or an acid solution containing metal ions with the phosphogypsum to prepare a suspension with the solid content of 0.01-0.1g/mL, carrying out crystal transformation reaction at 86-120 ℃ under normal pressure and stirring, carrying out solid-liquid separation after the reaction is finished, washing the solid by hot water and absolute ethyl alcohol in sequence, and drying to prepare the anhydrous gypsum, wherein the mass concentration of sulfuric acid in the acid solution containing the metal ions is 1-7%, the mass concentration of phosphoric acid calculated by phosphorus pentoxide is 30-50%, and the concentration of metal ions is 0.01-0.1mol/L; the method does not need any pretreatment such as desulfurization, impurity removal and the like, does not need calcination, has mild reaction conditions and simple operation, can realize the large-scale recycling of the phosphogypsum, and is suitable for industrial production and market popularization and application.
Description
Technical Field
The invention belongs to the technical field of preparation of inorganic functional materials, and particularly relates to a method for directly preparing anhydrous gypsum by using phosphogypsum in an acid solution system.
Background
Phosphogypsum is calcium sulfate solid waste discharged in the process of producing phosphoric acid by a wet method, usually exists in the form of calcium sulfate dihydrate and is used for producing 1 ton of P 2 O 5 About 4.5 to 5.5 tons of phosphogypsum are discharged. Compared with natural gypsum, the phosphogypsum usually contains phosphorus, fluorine, organic matters and the like, which influence the applicability of the phosphogypsum and increase the utilization cost of the phosphogypsum, and the phosphogypsum is mainly stockpiled at present. With the rapid development of the phosphorus chemical industry in China, the discharge amount of the phosphogypsum is increased year by year, and the pollution to soil and water sources caused by the phosphogypsum is also deepened year by year. The problem of phosphogypsum has become a world problem which seriously restricts the sustainable development and the environmental protection of the phosphorus chemical industry. The utilization modes of the phosphogypsum at home and abroad mainly include calcining to prepare building gypsum and preparing alpha high-strength gypsum by pressurized steam, and the two methods for utilizing the phosphogypsum have the defects of high production cost and relatively poor product performance. The problem of the field of recycling of phosphogypsum is always solved by finding a method which can utilize phosphogypsum at low cost and convert the phosphogypsum into a product with high added value.
The traditional anhydrous calcium sulfate usually adopts natural gypsum or phosphogypsum as a raw material, and water in the raw material is removed under the condition of heating, so that the anhydrous calcium sulfate is obtained. However, natural gypsum or phosphogypsum is produced from gypsum (CaSO) 4 ·2H 2 O) into plaster of paris (2 CaSO) 4 ·H 2 O is CaSO 4 ·1/2H 2 O), the calcium sulfate needs to be heated to 150-170 ℃, and the calcium sulfate needs to be heated to about 400 ℃ to be completely changed into anhydrous calcium sulfate. Therefore, the traditional calcining method for preparing the anhydrous calcium sulfate has higher energy consumption and cost, and is not beneficial to the anhydrous calcium sulfateLarge scale processing and wide range of applications.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for directly preparing anhydrous gypsum by using phosphogypsum, which has the characteristics of mild reaction conditions, simple process, low energy consumption, low cost and the like and is suitable for industrial production.
The method for directly preparing the anhydrous gypsum by using the phosphogypsum comprises the following steps:
(1) Preparation of acid solution containing metal ions
Mixing phosphoric acid, sulfuric acid and water to prepare a solution with the mass concentration of the sulfuric acid being 1-7% and the mass concentration of the phosphoric acid being 30-50% in terms of phosphorus pentoxide;
or metal oxide can be added into the solution to prepare an acid solution containing metal ions with the concentration of 0.01 to 0.1mol/L;
(2) Mixing phosphogypsum and an acid solution containing metal ions to prepare a suspension with the solid content of 0.01-0.1g/mL, carrying out crystal transformation reaction for 1.5-6 h at the temperature of 86-120 ℃ under normal pressure and stirring, carrying out solid-liquid separation, washing the solid with hot water and absolute ethyl alcohol in sequence, and drying to prepare anhydrous gypsum, wherein the liquid is reused for crystal transformation reaction.
The particle size of the phosphogypsum is 2 to 200 mu m.
The stirring speed is 80 to 320 r/min, the mixture is washed for 2 to 3 times by using ultrapure water at the temperature of 70 to 90 ℃, and then the mixture is washed by using absolute ethyl alcohol.
The invention has the beneficial effects that:
the method for preparing the anhydrous gypsum based on the phosphogypsum directly prepares the anhydrous gypsum by adopting a one-step method, does not need any pretreatment such as desulfurization, impurity removal and the like, does not need calcination, has mild reaction conditions and simple operation, can realize the large-scale reclamation of the phosphogypsum, and is suitable for industrial production and market popularization and application.
Drawings
FIG. 1 is an XRD pattern of anhydrite prepared under conditions of 0.05g/mL solids content in example 4;
FIG. 2 is an SEM photograph of anhydrite prepared under the condition of 0.05g/mL of solid content in example 4;
FIG. 3 is an SEM photograph of anhydrous gypsum obtained in example 5;
FIG. 4 is an SEM photograph of anhydrite obtained in example 6;
FIG. 5 is an SEM photograph of anhydrous gypsum obtained in example 7.
Detailed Description
The present invention is not limited to the following embodiments, and those skilled in the art can implement the present invention in other embodiments according to the disclosure of the present invention, or make simple changes or modifications on the design structure and idea of the present invention, and fall into the protection scope of the present invention. It should be noted that, in the present invention, the features of the examples and the features of the examples can be combined with each other without conflict, the phosphoric acid concentration is calculated by phosphorus pentoxide in the following examples, and the median particle size of phosphogypsum is 35.15 μm;
example 1
(1) Mixing concentrated phosphoric acid (85%), concentrated sulfuric acid (98%) and water to prepare an acid solution, wherein the mass concentration of the phosphoric acid in the acid solution is 38% and the mass solubility of the sulfuric acid is 5%;
(2) Putting phosphogypsum into an acid solution to prepare a suspension with the solid content of 0.1 g/mL;
(3) Adding stirring paddle into the suspension, stirring at 120 r/min, and maintaining at 85 deg.C, 88 deg.C, 94 deg.C, 100 deg.C, and 110 deg.C for 4.5h; the reaction product is filtered when the reaction product is hot, washed by hot water at 80 ℃ for 3 times, washed by absolute ethyl alcohol for 1 time, and finally dried at 50 ℃, and the result shows that no anhydrous gypsum is generated in the reaction at 85 ℃, and the anhydrous gypsum with the purity of 12.7%, 93.2%, 93.7% and 94.1% can be obtained in the reaction under other temperature conditions.
Example 2
(1) Mixing concentrated phosphoric acid (85%), concentrated sulfuric acid (98%) and water to prepare an acid solution, wherein the mass concentration of the phosphoric acid in the acid solution is 30%, and the mass concentration of the sulfuric acid is respectively 1%, 3%, 5%, 7% and 11%;
(2) Adding phosphogypsum into an acid solution to prepare a suspension with the solid content of 0.05 g/mL;
(3) Adding a stirring paddle into the suspension, stirring at the rotating speed of 120 r/min, preserving heat for 4.5 hours at 94 ℃, filtering the reaction product while the reaction product is hot, washing the reaction product with hot water at 80 ℃ for 3 times, washing the reaction product with absolute ethyl alcohol for 1 time, and finally drying the reaction product at 50 ℃ to obtain the anhydrous gypsum with the purity of 78.9 percent, 79.3 percent, 93.2 percent, 92.3 percent and 81.7 percent respectively.
Example 3
(1) Mixing concentrated phosphoric acid (85%), concentrated sulfuric acid (98%) and water to prepare an acid solution, wherein the mass concentration of the sulfuric acid in the acid solution is 5%, and the mass concentrations of the phosphoric acid are respectively 25%, 30%, 38%, 45% and 50%;
(2) Putting phosphogypsum into an acid solution to prepare a suspension with the solid content of 0.05 g/mL;
(3) Adding a stirring paddle into the suspension, stirring at the rotating speed of 120 r/min, preserving heat for 4.5 hours at 94 ℃, filtering the reaction product while the reaction product is hot, washing the reaction product with hot water at 80 ℃ for 3 times, washing the reaction product with absolute ethyl alcohol for 1 time, and finally drying the reaction product at 50 ℃, wherein the experimental result shows that when the mass concentration of the phosphoric acid is 25 percent, the anhydrous gypsum is not generated, and the anhydrous gypsum with the purity of 2.7 percent, 93.2 percent, 94.1 percent and 94.7 percent is respectively obtained under other concentration conditions.
Example 4
(1) Mixing concentrated phosphoric acid (85%), concentrated sulfuric acid (98%) and water to prepare an acid solution, wherein the mass concentration of the sulfuric acid in the acid solution is 5%, and the mass concentration of the phosphoric acid is 38%;
(2) Putting phosphogypsum into an acid solution to respectively prepare turbid liquids with solid contents of 0.01, 0.03, 0.05, 0.07, 0.09 and 0.15 g/mL;
(3) Adding a stirring paddle into the suspension, stirring at the rotating speed of 120 r/min, preserving heat for 4.5 hours at 94 ℃, filtering the reaction product while the reaction product is hot, washing the reaction product for 3 times by hot water at 80 ℃, washing the reaction product for 1 time by absolute ethyl alcohol, and finally drying the reaction product at 50 ℃, wherein the results show that when the solid content is 0.15g/mL, the fluidity is poor due to flocculation of the reactant, the subsequent treatment is difficult to separate solid from liquid, and the anhydrous gypsum with the purities of 35.5%, 93.2%, 92.8% and 91.7% is obtained under the condition of other solid contents, wherein the anhydrous gypsum prepared under the condition of the solid content of 0.05g/mL is shown in an XRD (X ray diffraction) diagram 1 and an SEM (SEM) diagram 2, the characteristic peak of the anhydrous calcium sulfate is extremely obvious and the purity is high in the diagram 1, and the particles in the anhydrous gypsum are uniformly distributed and the crystal morphology is relatively regular in the diagram 2.
Example 5
(1) Mixing concentrated phosphoric acid (85%), concentrated sulfuric acid (98%), magnesium oxide and water to prepare an acid solution containing magnesium ions, wherein the concentration of the magnesium ions is 0.09mol/L, the mass concentration of the phosphoric acid is 38% and the mass solubility of the sulfuric acid is 5%;
(2) Putting phosphogypsum into an acid solution containing magnesium ions to prepare a suspension with the solid content of 0.05 g/mL;
(3) Adding a stirring paddle into the suspension, stirring at a rotating speed of 120 r/min, and keeping the temperature at 94 ℃ for 4 hours; filtering the reaction product while hot, washing with 80 deg.C hot water for 3 times, washing with anhydrous ethanol for 1 time, and drying at 50 deg.C to obtain anhydrous gypsum with purity of 94.2%, wherein the anhydrous gypsum has SEM figure 3, and compared with figure 2, the anhydrous gypsum crystal is more fine and has more needle and rod crystal forms.
Example 6
(1) Mixing concentrated phosphoric acid (85%), concentrated sulfuric acid (98%), alumina and water to obtain a mixture with an aluminum ion concentration of 0.09mol/L,
An acid solution with the phosphoric acid mass concentration of 38% and the sulfuric acid mass solubility of 5%;
(2) Putting phosphogypsum into an acid solution containing aluminum ions to prepare a suspension with the solid content of 0.05 g/mL;
(3) Adding a stirring paddle into the suspension, stirring at the rotating speed of 120 r/min, and preserving heat for 4.5 hours at 94 ℃; and (3) filtering the reaction product while the reaction product is hot, washing the reaction product with hot water at 80 ℃ for 3 times, washing the reaction product with absolute ethyl alcohol for 1 time, and finally drying the reaction product at 50 ℃ to obtain the anhydrous gypsum with the purity of 92.7 percent, wherein an SEM picture of the anhydrous gypsum is shown in figure 4, and compared with figure 2, the anhydrous gypsum has obvious needle-like crystal form and crystals become thicker and longer after aluminum ions are added.
Example 7
(1) Mixing concentrated phosphoric acid (85%), concentrated sulfuric acid (98%), iron oxide and water to obtain a mixture with iron ion concentration of 0.09mol/L,
An acid solution with the phosphoric acid mass concentration of 38% and the sulfuric acid mass solubility of 5%;
(2) Putting phosphogypsum into an acid solution containing iron ions to prepare a suspension with a solid content of 0.05 g/mL;
(3) Adding a stirring paddle into the suspension, stirring at a rotating speed of 120 r/min, and keeping the temperature at 94 ℃ for 4.5 hours; and (3) filtering the reaction product while the reaction product is hot, washing the reaction product with hot water at 80 ℃ for 3 times, washing the reaction product with absolute ethyl alcohol for 1 time, and finally drying the reaction product at 50 ℃ to obtain the anhydrous gypsum with the purity of 91.8 percent, wherein an SEM picture of the anhydrous gypsum is shown in a figure 4, and compared with a figure 2, the needle-like crystal form of the anhydrous gypsum after the iron ions are added is obvious and regular.
Claims (6)
1. A method for directly preparing anhydrous gypsum by using phosphogypsum is characterized by comprising the following steps: mixing an acid solution and phosphogypsum to prepare a suspension with the solid content of 0.01-0.1g/mL, carrying out crystal transformation reaction at 86-120 ℃ under normal pressure and stirring, carrying out solid-liquid separation after the reaction is finished, washing the solid with hot water and absolute ethyl alcohol in sequence, and drying to prepare the anhydrous gypsum, wherein the mass concentration of sulfuric acid in the acid solution containing metal ions is 1-7%, and the mass concentration of phosphoric acid calculated by phosphorus pentoxide is 30-50%.
2. The method for directly preparing the anhydrous gypsum by using the phosphogypsum according to claim 1, which is characterized in that: the acid solution contains metal ions, and the concentration of the metal ions is 0.01 to 0.1mol/L.
3. The method for directly preparing the anhydrous gypsum by using the phosphogypsum according to claim 1, which is characterized in that: the particle size of the phosphogypsum is 2 to 200 mu m.
4. The method for directly preparing anhydrous gypsum by using phosphogypsum according to claim 1, characterized in that: the metal ions are selected from one or more of sodium ions, magnesium ions, aluminum ions and iron ions.
5. The method for directly preparing the anhydrous gypsum by using the phosphogypsum according to claim 1, which is characterized in that: the temperature of the washing hot water is 70 to 90 ℃, and the drying temperature is 40 to 60 ℃.
6. The method for directly preparing anhydrous gypsum by using phosphogypsum according to claim 1, characterized in that: the crystal transformation reaction time is 1.5 to 6h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117886526A (en) * | 2024-01-26 | 2024-04-16 | 湖北省长江资源循环利用及装备创新中心有限公司 | Method for preparing II-type anhydrous gypsum and building gypsum from phosphogypsum |
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| CN106430273A (en) * | 2016-09-30 | 2017-02-22 | 四川什邡市星天丰科技有限公司 | Method for preparing anhydrous calcium sulfate filler by using phosphogypsum |
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| CN117886526A (en) * | 2024-01-26 | 2024-04-16 | 湖北省长江资源循环利用及装备创新中心有限公司 | Method for preparing II-type anhydrous gypsum and building gypsum from phosphogypsum |
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