CN114229877A - Method for decomposing phosphogypsum at low temperature - Google Patents

Method for decomposing phosphogypsum at low temperature Download PDF

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CN114229877A
CN114229877A CN202210000610.6A CN202210000610A CN114229877A CN 114229877 A CN114229877 A CN 114229877A CN 202210000610 A CN202210000610 A CN 202210000610A CN 114229877 A CN114229877 A CN 114229877A
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phosphogypsum
decomposition
introducing
temperature
low temperature
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邓秋林
罗琴
郭礼清
黄晓枫
董发勤
谭宏斌
雷琴
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Southwest University of Science and Technology
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    • 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
    • C01F11/02—Oxides or hydroxides
    • C01F11/04—Oxides or hydroxides by thermal decomposition
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
    • 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
    • C04B2/00—Lime, magnesia or dolomite
    • C04B2/005—Lime, magnesia or dolomite obtained from an industrial by-product

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Abstract

The invention provides a method for decomposing phosphogypsum at low temperature, and belongs to the technical field of phosphorus chemical treatment. The specific scheme is as follows: pretreating phosphogypsum in a metal ion solution, putting the dried phosphogypsum into a tube furnace, introducing CO in a nitrogen atmosphere, and introducing the CO at 500-900 DEG CoAnd C, reducing the phosphogypsum into CaS, and then switching oxygen to oxidize the CaS into CaO so as to realize low-temperature decomposition of the phosphogypsum. The method has the advantages of low decomposition temperature, wide application prospect and the like.

Description

Method for decomposing phosphogypsum at low temperature
Technical Field
The invention relates to a method for decomposing phosphogypsum at low temperature, in particular to the method for decomposing the phosphogypsum by two steps, which has simple process and lower decomposition temperature and belongs to the technical field of phosphorus chemical treatment.
Background
Phosphogypsum is a solid waste generated by the reaction of sulfuric acid and phosphate ore in the production process of industrial wet-process phosphoric acid, and the main component of the phosphogypsum is calcium sulfate dihydrate (CaSO)4·2H2O), the impurities are mainly SiO2、P2O5F compounds, and metal oxides such as Mg and Al. China is used as the first country for producing large phosphate fertilizers and the first country for producing phosphogypsum as a byproduct in the world, and about 4-5 tons of phosphogypsum are produced in each 1 ton of phosphoric acid prepared in the wet-process phosphoric acid production process. While the phosphorization industry is rapidly developed, the phosphogypsum also becomes a problem which is difficult to solve in the industry. The accumulated amount of phosphogypsum in China exceeds 7 hundred million tons, the annual emission amount is up to 8000 ten thousand tons, and the utilization rate is less than 40 percent. Most phosphogypsum is directly piled in the open air or poured into the sea, which not only causes resource waste and environmental pollution, but also influences social development and threatens human safety. The phosphogypsum is widely applied to the aspects of building materials, chemical products, agricultural production and the like at present, wherein the most consumed phosphogypsum is decomposed to prepare CaO and coproduce sulfuric acid. The technical problems of high decomposition energy consumption, high decomposition temperature, large investment economic cost, unsatisfactory later-period economic benefit and the like of the phosphogypsum need to be improved. Therefore, lowering the decomposition temperature of phosphogypsum and increasing the benefit are the most important research directions at present.
The invention patent CN101357773B discloses a method for reducing the decomposition temperature of phosphogypsum, which comprises respectively using gaseous reducing agents CO and H2S, adding powder of solid reducing agents such as fly ash, coal gangue and the like and gas-solid, solid-solid composite reducing agents serving as additives into phosphogypsum for decomposition, adopting double-atmosphere reaction to reduce the decomposition temperature of the phosphogypsum and ensure high decomposition rate and desulfurization rate, and reducing the decomposition temperature of the phosphogypsum to be less than or equal to 1000oC, decomposition rate is more than or equal to 95 percent, and SO can be stably recovered2And (4) resources.
The invention patent CN101186281B discloses a method for reducing the decomposition temperature of phosphogypsum in the process of producing acid by phosphogypsum, coal is used as a reducing agent in the process of producing acid by phosphogypsum and co-producing cement clinker, and MgO, NaCl and SiO are added2、Al2O3、Fe2O3A composite catalyst as main component, which is prepared from ardealiteThe decomposition temperature is reduced to 700-750 deg.CoC, energy consumption is reduced, and the generated calcium compound can be directly used as high-quality cement clinker and SO2Can be directly used as acid-making raw materials.
The invention patent CN105036170A discloses a method for preparing calcium oxide by decomposing phosphogypsum, which decomposes and generates CaO in a reducing atmosphere-oxidizing atmosphere for two times in a circulating way, and the generated CaO can be used as a filling agent and a drying agent to prepare calcium carbide, soda ash, bleaching powder and the like.
The invention patent CN101456542A discloses a method for reductive decomposition of phosphogypsum by carbon monoxide at a temperature of 750-850 DEG CoC，N2Introducing CO to reduce and decompose the phosphogypsum under the atmosphere. SO in tail gas2The volume percentage content is more than or equal to 10 percent, the solid slag material can be directly used as qualified raw material gas for producing sulfuric acid by the two-conversion and two-absorption acid making process, the solid slag material component is more than or equal to 70 weight percent of CaO, and the solid slag material can be used as cement clinker.
The invention patent CN103466675A discloses a method for decomposing phosphogypsum at low temperature, which uses Fe-Ni composite catalysis to decompose phosphogypsum under the atmosphere of carbon monoxide, and reduces the decomposition temperature of the phosphogypsum to 570-630%oC, the aim of saving energy and reducing consumption is achieved, the generated CaO can be used as high-quality cement clinker, and the generated SO2Can be used as raw material gas for preparing acid.
The prior phosphogypsum decomposition technology generally has the following problems: higher decomposition temperature, complex decomposition process, more product components, lower product yield and high energy consumption. If the method can simplify the operation steps, increase the product yield and simplify the product components on the basis of reducing the decomposition temperature of the phosphogypsum, create conditions for the resource utilization of the phosphogypsum and increase the recovery utilization rate of resources.
Disclosure of Invention
The invention provides a simple and effective method for decomposing phosphogypsum at low temperature. The method takes carbon monoxide as a reducing gas and ferric chloride, cobalt chloride and nickel chloride as catalytic auxiliaries, and reduces the decomposition temperature of phosphogypsum to 500-900 DEG CoAnd C, simplifying operation steps, improving the decomposition rate and improving the product purity.
The patent aims to provide a method for decomposing phosphogypsum at low temperature, which is characterized by comprising the following steps:
(1) crushing, grinding and sieving the phosphogypsum.
(2) Soaking the screened 100-120-mesh phosphogypsum powder in a metal ion impregnation liquid, and stirring for 8-12 h, wherein the metal ion impregnation liquid contains Fe3+、Co2+、Ni2+At least one of (1) in the impregnating solution, Fe3+The concentration of (A) is 0.4 to 0.8 mol/L, Co2+The concentration of (A) is 0.4 to 0.6 mol/L, Ni2+The concentration of the filter residue is 0.4-0.6 mol/L, and the filtered filter residue is 110-130 mol/LoAnd C, drying for 1-2 h to obtain the pretreated phosphogypsum.
(3) And (3) putting the phosphogypsum obtained in the step (2) into a tube furnace, and introducing nitrogen for 3-5 min. Switching the gas to CO with the purity of 99.99 percent and decomposing at the temperature of 500-900 DEG CoCalcining for 30-120 min under C, and reducing the phosphogypsum into CaS.
(4) And (4) after the step (3) is finished, switching the gas in the tubular furnace into oxygen at the decomposition temperature, and introducing for 30-90 min to oxidize the CaS into CaO.
The phosphogypsum has complex components, more byproducts, complex decomposition mechanism, high heat absorption and high decomposition temperature in the decomposition process. Under the reducing atmosphere, the addition of metal ions can reduce the decomposition temperature of the phosphogypsum and promote the decomposition of the phosphogypsum; the method decomposes the phosphogypsum into calcium sulfide and then converts the calcium sulfide into calcium oxide, so that the decomposition temperature of the phosphogypsum can be reduced, the energy required by decomposition is reduced, and the operation is simple and easy. Under the atmosphere of quantitative CO reduction, metal ion catalysis is adopted, and the solution containing metal ions used in the experiment is Fe3+、Co2+、Ni2+At least one of the above-mentioned materials is used for decomposing phosphogypsum by steps by switching gas required by reaction, and the main products obtained by experiment are CaO and SO2。
In a CO reduction atmosphere, decomposing phosphogypsum by adopting metal ions after dipping and then oxidizing, wherein the main reaction in the process is as follows:
Figure RE-333965DEST_PATH_IMAGE001
Figure RE-276513DEST_PATH_IMAGE002
Figure RE-356858DEST_PATH_IMAGE003
Figure RE-777475DEST_PATH_IMAGE004
Figure RE-984466DEST_PATH_IMAGE005
the phosphogypsum is solid waste generated by a wet-process phosphoric acid process, and the main components of the phosphogypsum are shown in a table 1:
table 1: main component of phosphogypsum raw material
Composition (I) Content (%) Composition (I) Content (%)
SO3 49.77 Fe2O3 0.13
CaO 41.29 BaO 0.1
SiO2 5.99 SrO 0.09
P2O5 0.94 Na2O 0.07
F 0.86 K2O 0.06
Al2O3 0.67 MgO 0.02
The device for decomposing phosphogypsum at low temperature is shown in the attached drawing.
The invention has the beneficial effects that:
(1) the method has simple process and low energy consumption, and reduces the decomposition temperature of the phosphogypsum to 500-900 DEG CoC。
(2) The present patent proposes a new metal ion catalyst system.
（3）Fe3+、Co2+、Ni2+Are all common metal ions, and the amount of the catalyst used is small,
(4) the method provided by the invention is beneficial to reducing the temperature in the process of preparing CaO and co-producing cement by decomposing phosphogypsum, and has wide application prospect.
Drawings
FIG. 1 is a diagram of an experimental apparatus of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples, but the scope of the present invention is not limited to the examples.
In the description of the embodiments of the present invention, it is to be understood that "-" and "-" denote ranges of two numerical values, and the ranges include endpoints. For example: "A-B" means a range of greater than or equal to A and less than or equal to B. "A to B" means a range of not less than A and not more than B.
In the description of the embodiments of the present invention, the term "and/or" herein is only one kind of association relationship describing an associated object, and means that there may be three kinds of relationships, for example, a and/or B, and may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Example 1:
the phosphogypsum is crushed, ground and sieved by a 100-mesh sieve. Soaking the screened phosphogypsum powder in ferric chloride solution (Fe)3+0.8 mol/L) for 12 hours, and filtering residue after filtration is at 110oAnd C, drying for 2 h to obtain the pretreated phosphogypsum. Putting the pretreated phosphogypsum into a tube furnace, introducing CO with the purity of 99.99 percent under the protection of nitrogen, and introducing the CO into the tube furnace at 900 DEGoCalcining for 1 h at the temperature of C, introducing CO gas and CaSO in phosphogypsum4The molar ratio is 3.5:1, and the phosphogypsum is reduced into CaS. And after the steps are finished, switching the gas in the tubular furnace to oxygen, and introducing for 30 min for oxidation. After the reaction, the reaction mixture was cooled to room temperature and the S content in the residue was measured by iodometry2-And (4) calculating the desulfurization rate by using a flue gas analyzer, and then calculating the amount of calcium sulfate and calcium sulfide in the residue. The decomposition rate of phosphogypsum can be calculated according to the following formula:
Figure RE-97915DEST_PATH_IMAGE006
the determination and calculation result shows that the decomposition rate of the phosphogypsum in the embodiment is 95.9 percent, and the content of calcium sulfide in the residue is 29.2 percent.
Example 2:
the phosphogypsum is crushed, ground and sieved by a 100-mesh sieve. Soaking the screened phosphogypsum powder in cobalt chloride solution (Co)2+0.6 mol/L) for 12 hours, and filtering residue after filtration is at 110oAnd C, drying for 2 h to obtain the pretreated phosphogypsum. Placing the pretreated phosphogypsum into a tube furnaceIntroducing CO with the purity of 99.99 percent under the protection of nitrogen, and introducing the CO at 900 DEG CoCalcining for 1 h at the temperature of C, introducing CO gas and CaSO in phosphogypsum4The molar ratio is 3.5:1, and the phosphogypsum is reduced into CaS. And after the steps are finished, switching the gas in the tubular furnace to oxygen, and introducing for 30 min for oxidation. After the reaction, the reaction mixture was cooled to room temperature and the S content in the residue was measured by iodometry2-And (4) calculating the desulfurization rate by using a flue gas analyzer, and then calculating the amount of calcium sulfate and calcium sulfide in the residue. The decomposition rate of phosphogypsum can be calculated according to the following formula:
Figure RE-23146DEST_PATH_IMAGE006
the determination and calculation result shows that the decomposition rate of the phosphogypsum in the embodiment is 95.4 percent, and the content of calcium sulfide in the residue is 29.3 percent.
Example 3:
the phosphogypsum is crushed, ground and sieved by a 100-mesh sieve. Soaking the screened phosphogypsum powder in nickel chloride solution (Ni)2+0.6 mol/L) for 12 hours, and filtering residue after filtration is at 110oAnd C, drying for 2 h to obtain the pretreated phosphogypsum. Putting the pretreated phosphogypsum into a tube furnace, introducing CO with the purity of 99.99 percent under the protection of nitrogen, and introducing the CO into the tube furnace at 900 DEGoCalcining for 1 h at the temperature of C, introducing CO gas and CaSO in phosphogypsum4The molar ratio is 3.5:1, and the phosphogypsum is reduced into CaS. And after the steps are finished, switching the gas in the tubular furnace to oxygen, and introducing for 30 min for oxidation. After the reaction, the reaction mixture was cooled to room temperature and the S content in the residue was measured by iodometry2-And (4) calculating the desulfurization rate by using a flue gas analyzer, and then calculating the amount of calcium sulfate and calcium sulfide in the residue. The decomposition rate of phosphogypsum can be calculated according to the following formula:
Figure RE-388399DEST_PATH_IMAGE006
the determination and calculation result shows that the decomposition rate of the phosphogypsum in the embodiment is 96.3 percent, and the content of calcium sulfide in the residue is 29.2 percent.
Example 4:
the phosphogypsum is crushed, ground and sieved by a sieve with 110 meshes. Immersing the screened phosphogypsum powder in a solution (Fe) containing ferric chloride and cobalt chloride3+Has a concentration of 0.6 mol/L, Co2+0.5 mol/L) for 11 hours, and filtering residue after filtration is 120oAnd C, drying for 2 h to obtain the pretreated phosphogypsum. Putting the pretreated phosphogypsum into a tube furnace, introducing CO with the purity of 99.99 percent under the protection of nitrogen, and reacting at 800 DEG CoCalcining for 1 h at the temperature of C, introducing CO gas and CaSO in phosphogypsum4Reducing the phosphogypsum into CaS with the molar ratio of 4: 1. And after the steps are finished, switching the gas in the tubular furnace to oxygen, and introducing for 60 min for oxidation. After the reaction, the reaction mixture was naturally cooled to room temperature, and S in the residue was measured by iodometry2-And (4) calculating the desulfurization rate by using a flue gas analyzer, and then calculating the amount of calcium sulfate and calcium sulfide in the residue. The decomposition rate of phosphogypsum can be calculated according to the following formula:
Figure RE-449896DEST_PATH_IMAGE006
the determination and calculation result shows that the decomposition of the phosphogypsum in the embodiment is 96.1 percent, and the content of calcium sulfide in the residue is 28.9 percent.
Example 5:
the phosphogypsum is crushed, ground and sieved by a sieve with 110 meshes. Immersing the screened phosphogypsum powder in a solution (Fe) containing ferric chloride and nickel chloride3+Has a concentration of 0.6 mol/L, Ni2+0.5 mol/L) for 11 hours, and filtering residue after filtration is 120oAnd C, drying for 2 h to obtain the pretreated phosphogypsum. Putting the pretreated phosphogypsum into a tube furnace, introducing CO with the purity of 99.99 percent under the protection of nitrogen, and reacting at 800 DEG CoCalcining for 1 h at the temperature of C, introducing CO gas and CaSO in phosphogypsum4Reducing the phosphogypsum into CaS with the molar ratio of 4: 1. And after the steps are finished, switching the gas in the tubular furnace to oxygen, and introducing for 60 min for oxidation. After the reaction is finished, naturally cooling to room temperature,iodometric determination of S in the residue2-And (4) calculating the desulfurization rate by using a flue gas analyzer, and then calculating the amount of calcium sulfate and calcium sulfide in the residue. The decomposition rate of phosphogypsum can be calculated according to the following formula:
Figure RE-734247DEST_PATH_IMAGE006
the decomposition of the phosphogypsum in the embodiment is 95.4 percent and the content of calcium sulfide in the residue is 29 percent through measurement and calculation.
Example 6:
the phosphogypsum is crushed, ground and sieved by a sieve with 110 meshes. Immersing the screened phosphogypsum powder in a solution (Co) containing cobalt chloride and nickel chloride2+Has a concentration of 0.5 mol/L, Ni2+0.5 mol/L) for 11 hours, and filtering residue after filtration is 120oAnd C, drying for 2 h to obtain the pretreated phosphogypsum. Putting the pretreated phosphogypsum into a tube furnace, introducing CO with the purity of 99.99 percent under the protection of nitrogen, and reacting at 800 DEG CoCalcining for 1 h at the temperature of C, introducing CO gas and CaSO in phosphogypsum4Reducing the phosphogypsum into CaS with the molar ratio of 4: 1. And after the steps are finished, switching the gas in the tubular furnace to oxygen, and introducing for 60 min for oxidation. After the reaction, the reaction mixture was naturally cooled to room temperature, and S in the residue was measured by iodometry2-And (4) calculating the desulfurization rate by using a flue gas analyzer, and then calculating the amount of calcium sulfate and calcium sulfide in the residue. The decomposition rate of phosphogypsum can be calculated according to the following formula:
Figure RE-458358DEST_PATH_IMAGE006
the decomposition of phosphogypsum in the example is 95.7% and the content of calcium sulfide in the residue is 28.5% through measurement and calculation.
Example 7:
the phosphogypsum is crushed, ground and sieved by a 120-mesh sieve. Immersing the screened phosphogypsum powder in a solution (Fe) containing ferric chloride, nickel chloride and cobalt chloride3+Has a concentration of 0.4 mol/L、Co2+Has a concentration of 0.4 mol/L, Ni2+0.4 mol/L) for 10 hours, and filtering residue after filtration is put in a stirring tank of 130oAnd C, drying for 2 h to obtain the pretreated phosphogypsum. Putting the pretreated phosphogypsum into a tube furnace, introducing CO with the purity of 99.99 percent under the protection of nitrogen, and introducing the CO into the tube furnace at 700 DEGoCalcining for 1 h at the temperature of C, introducing CO gas and CaSO in phosphogypsum4The molar ratio is 4.5:1, and the phosphogypsum is reduced into CaS. And after the steps are finished, switching the gas in the tubular furnace to oxygen, and introducing for 90 min for oxidation. After the reaction, the reaction mixture was naturally cooled to room temperature, and S in the residue was measured by iodometry2-And (4) calculating the desulfurization rate by using a flue gas analyzer, and then calculating the amount of calcium sulfate and calcium sulfide in the residue. The decomposition rate of phosphogypsum can be calculated according to the following formula:
Figure RE-486357DEST_PATH_IMAGE006
the decomposition of phosphogypsum in the example is 97.1% and the content of calcium sulfide in the residue is 27.3% through measurement and calculation.

Claims (4)

1. A method for decomposing phosphogypsum at low temperature mainly comprises the following steps:
(1) crushing, grinding and sieving the phosphogypsum.
(2) Soaking phosphogypsum powder in a soaking solution containing metal ions, stirring for 8-12 h, and filtering to obtain filter residues at 110-130%oAnd C, drying to obtain the pretreated phosphogypsum.
(3) And (3) putting the phosphogypsum obtained in the step (2) into a tube furnace, and introducing nitrogen for 3-5 min. And switching gas to CO, calcining for 30-90 min at a certain decomposition temperature, and reducing phosphogypsum to CaS.
(4) And (4) after the step (3) is finished, switching to oxygen in the tubular furnace, and introducing for 30-120 min to oxidize the CaS into CaO.
2. The process of low temperature decomposition of phosphogypsum according to claim 1, characterized in that in step (2) the metal is containedThe ion impregnation liquid contains Fe3+、Co2+、Ni2+At least one of (1).
3. The method for decomposing phosphogypsum at low temperature according to claim 1, wherein the decomposition temperature of the phosphogypsum in the step (3) is 500-900 ~oC。
4. The method of claim 1, wherein the CO gas is introduced with the CaSO in phosphogypsum4The molar ratio is 3.5-4.5: 1.
CN202210000610.6A 2022-01-04 2022-01-04 Method for decomposing phosphogypsum at low temperature Pending CN114229877A (en)

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Publication number Priority date Publication date Assignee Title
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CN103408052A (en) * 2013-07-25 2013-11-27 昆明理工大学 Decomposition method of ardealite
CN103466675A (en) * 2013-09-03 2013-12-25 昆明理工大学 Decomposition method of ardealite
CN105036170A (en) * 2015-07-27 2015-11-11 昆明理工大学 Method for preparing calcium oxide through phosphogypsum decomposition
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