CN111170668A - Calcination treatment method of phosphogypsum and application of obtained phosphogypsum - Google Patents
Calcination treatment method of phosphogypsum and application of obtained phosphogypsum Download PDFInfo
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- CN111170668A CN111170668A CN202010026440.XA CN202010026440A CN111170668A CN 111170668 A CN111170668 A CN 111170668A CN 202010026440 A CN202010026440 A CN 202010026440A CN 111170668 A CN111170668 A CN 111170668A
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- phosphogypsum
- calcination treatment
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- 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
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- 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
- C04B11/02—Methods and apparatus for dehydrating gypsum
- C04B11/024—Ingredients added before, or during, the calcining process, e.g. calcination modifiers
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- 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
- C04B11/02—Methods and apparatus for dehydrating gypsum
- C04B11/028—Devices therefor characterised by the type of calcining devices used therefor or by the type of hemihydrate obtained
- C04B11/036—Devices therefor characterised by the type of calcining devices used therefor or by the type of hemihydrate obtained for the dry process, e.g. dehydrating in a fluidised bed or in a rotary kiln, i.e. to obtain beta-hemihydrate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a calcination treatment method of phosphogypsum and application of the obtained phosphogypsum, wherein the calcination treatment method comprises the following steps: (1) mixing phosphorus-and fluorine-containing phosphogypsum with an additive to obtain a mixture; (2) and (3) calcining the mixture obtained in the step (1) to obtain a phosphogypsum product. The method provided by the invention can be used for obtaining the phosphogypsum product meeting the first-level requirement in GB/T23456-2018 specification under the condition of low temperature and short-time calcination, and further can be directly used for preparing the calcined phosphogypsum.
Description
Technical Field
The invention relates to the field of phosphogypsum, in particular to a calcination treatment method of phosphogypsum.
Background
Phosphogypsum is an industrial waste residue discharged in the process of producing phosphoric acid by a chemical wet method, and the main component of the phosphogypsum is calcium sulfate dihydrate (CaSO)4·2H2O), is a potential gypsum resource. However, phosphogypsum has other impurities, especially water-soluble impurity ions such as phosphorus and fluorine, which can seriously limit the commercial and industrial application of phosphogypsum when the impurities exceed the minimum level. The water-soluble phosphorus forms Ca in the process of hydrating phosphogypsum3(PO4)2The gypsum is coated on the surface of the gypsum crystal, so that the setting time of the gypsum is prolonged, and the strength is reduced; water-soluble fluorine has an accelerating effect on gypsum, but when the content thereof exceeds 0.3%, the strength of gypsum is remarkably reduced.
Phosphogypsum pretreatment is an important means for phosphogypsum resource utilization, and the current phosphogypsum pretreatment methods mainly comprise a water washing method, a lime neutralization method, a flotation method, a ball milling method, a screening method and the like.
CN106977123A discloses a process method for removing impurity fluorine in phosphogypsum by adding water to citric acid, which utilizes chemical action of impurities in phosphogypsum citrate to convert impurities such as fluoride, phosphate and the like in phosphogypsum into soluble substances capable of being washed by water, and then removes impurities by a washing process, thereby reducing the content of fluoride in equipment and drying smoke. However, the process generates a large amount of fluorine-containing wastewater, needs secondary treatment and causes a certain degree of pollution to the environment. CN110563367A discloses a method for neutralizing, phosphorus fixing and fluorine fixing of phosphogypsum and the obtained phosphogypsum, wherein the acidic and soluble phosphorus and fluorine contents of the phosphogypsum are effectively reduced by using carbide slag to perform neutralization, phosphorus fixing and fluorine fixing treatment on the phosphogypsum, but the treatment time is long, and the method is not beneficial to industrial production.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a calcination treatment method of phosphogypsum and application of the obtained phosphogypsum, by which a phosphogypsum product meeting the first-class requirement in GB/T23456-2018 specification can be obtained under the condition of calcination at a lower temperature in a short time, and further can be directly used for preparing calcined phosphogypsum.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, a method of calcination treatment of phosphogypsum comprises the following steps:
(1) mixing phosphorus-and fluorine-containing phosphogypsum with an additive to obtain a mixture;
(2) and (3) calcining the mixture obtained in the step (1) to obtain a phosphogypsum product.
According to the method provided by the invention, the additive is added into the phosphogypsum containing phosphorus and fluorine and the phosphogypsum is calcined at low temperature, so that the phosphorus and the fluorine in the phosphogypsum are quickly inerted and removed at low temperature, and a phosphogypsum product meeting the first-class requirement in GB/T23456-2018 specification can be obtained, and further, the phosphogypsum can be directly used for preparing calcined phosphogypsum.
In a preferred embodiment of the present invention, the additive is added in the step (1) in an amount of 0.5 to 10% by mass, for example, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10% by mass, based on the mass of the phosphorus-and fluorine-containing phosphogypsum, but not limited to the above-mentioned values, and other values not listed in this range are also applicable.
As a preferred technical scheme of the invention, the additive in the step (1) comprises 1 or a combination of at least 2 of ammonium chloride, ammonium carbonate, ammonium bicarbonate, ammonium acetate, calcium chloride, calcium acetate or sodium acetate.
As a preferred technical scheme of the invention, the mixing mode in the step (1) comprises crushing and/or ball milling.
In a preferred embodiment of the present invention, the mixing time in the step (1) is 2 to 10min, for example, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10min, but not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
As a preferred embodiment of the present invention, the temperature of the calcination treatment in the step (2) is 140 to 210 ℃ and may be, for example, 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃, 200 ℃ or 210 ℃, but is not limited to the values listed, and other values not listed in the range are also applicable.
In a preferred embodiment of the present invention, the time for the calcination treatment in step (2) is 3 to 10 hours, and may be, for example, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, or 10 hours, but is not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
As a preferable technical scheme of the invention, the mixture in the step (1) is sieved;
preferably, the sieve has a mesh size of 100 mesh;
preferably, the sieved undersize product is used for the calcination treatment of step (2).
As a preferred technical scheme of the invention, the calcination treatment comprises the following steps:
(1) mixing phosphorus-and fluorine-containing phosphogypsum with an additive for 2-10min to obtain a mixture; wherein the additive amount is 0.5-10% of the phosphorus and fluorine-containing phosphogypsum by mass; the additive comprises 1 or a combination of at least 2 of ammonium chloride, ammonium carbonate, ammonium bicarbonate, ammonium acetate, calcium chloride, calcium acetate, or sodium acetate; the mixing mode comprises crushing and/or ball milling;
(2) calcining the mixture obtained in the step (1) at 140-210 ℃ for 3-10h to obtain a phosphogypsum product;
screening the mixture obtained in the step (1); the size of the screened sieve pore is 100 meshes;
the sieved undersize product is used for the calcination treatment of step (2).
Use of the phosphogypsum product obtained by the calcination treatment process according to the second aspect as described in the first aspect, for the preparation of calcined phosphogypsum.
Compared with the prior art, the invention has the following beneficial effects:
the method provided by the invention can be used for obtaining the phosphogypsum product meeting the first-level requirement in GB/T23456-2018 specification under the condition of low temperature and short-time calcination, and further can be directly used for preparing the calcined phosphogypsum.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides a calcination treatment method of phosphogypsum, which comprises the following steps of (1) mixing phosphogypsum containing phosphorus and fluorine with an additive for 5min to obtain a mixture; wherein the additive amount of the additive is 2 percent of the mass of the phosphorus and fluorine-containing phosphogypsum; the additive is ammonium chloride; the mixing mode comprises crushing;
(2) calcining the mixture obtained in the step (1) at 160 ℃ for 4h to obtain a phosphogypsum product;
and (3) carrying out soluble phosphorus and fluorine tests on the obtained phosphogypsum product, wherein the specific test process refers to GB/T23456-2018 phosphogypsum, and the specific test results are detailed in Table 1.
Example 2
The embodiment provides a calcination treatment method of phosphogypsum, which comprises the following steps of (1) mixing phosphogypsum containing phosphorus and fluorine with an additive for 10min to obtain a mixture; wherein the additive amount is 0.5 percent of the mass of the phosphorus and fluorine-containing phosphogypsum; the additive is ammonium carbonate; the mixing mode comprises crushing;
(2) calcining the mixture obtained in the step (1) at 140 ℃ for 3h to obtain a phosphogypsum product;
and (3) carrying out soluble phosphorus and fluorine tests on the obtained phosphogypsum product, wherein the specific test process refers to GB/T23456-2018 phosphogypsum, and the specific test results are detailed in Table 1.
Example 3
The embodiment provides a calcination treatment method of phosphogypsum, which comprises the following steps of (1) mixing phosphogypsum containing phosphorus and fluorine with an additive for 2min to obtain a mixture; wherein the additive amount is 1% of the phosphorus and fluorine-containing phosphogypsum by mass; the additive is ammonium acetate; the mixing manner comprises ball milling;
(2) calcining the mixture obtained in the step (1) at 170 ℃ for 4h to obtain a phosphogypsum product;
and (3) carrying out soluble phosphorus and fluorine tests on the obtained phosphogypsum product, wherein the specific test process refers to GB/T23456-2018 phosphogypsum, and the specific test results are detailed in Table 1.
Example 4
The embodiment provides a calcination treatment method of phosphogypsum, which comprises the following steps of (1) mixing phosphogypsum containing phosphorus and fluorine with an additive for 8min to obtain a mixture; wherein the additive amount is 5% of the phosphorus and fluorine-containing phosphogypsum by mass; the additive is calcium chloride; the mixing manner comprises ball milling;
(2) calcining the mixture obtained in the step (1) at 160 ℃ for 4h to obtain a phosphogypsum product;
and (3) carrying out soluble phosphorus and fluorine tests on the obtained phosphogypsum product, wherein the specific test process refers to GB/T23456-2018 phosphogypsum, and the specific test results are detailed in Table 1.
Example 5
The embodiment provides a calcination treatment method of phosphogypsum, which comprises the following steps of (1) mixing phosphogypsum containing phosphorus and fluorine with an additive for 4min to obtain a mixture; wherein the additive amount is 3% of the phosphorus and fluorine-containing phosphogypsum by mass; the additive is sodium acetate; the mixing manner comprises ball milling;
(2) calcining the mixture obtained in the step (1) at 160 ℃ for 4h to obtain a phosphogypsum product;
and (3) carrying out soluble phosphorus and fluorine tests on the obtained phosphogypsum product, wherein the specific test process refers to GB/T23456-2018 phosphogypsum, and the specific test results are detailed in Table 1.
Example 6
The embodiment provides a calcination treatment method of phosphogypsum, which comprises the following steps of (1) mixing phosphogypsum containing phosphorus and fluorine with an additive for 7min to obtain a mixture; wherein the additive amount is 10% of the phosphorus and fluorine-containing phosphogypsum by mass; the additive is calcium acetate; the mixing manner comprises ball milling;
(2) calcining the mixture obtained in the step (1) at 160 ℃ for 4h to obtain a phosphogypsum product;
and (3) carrying out soluble phosphorus and fluorine tests on the obtained phosphogypsum product, wherein the specific test process refers to GB/T23456-2018 phosphogypsum, and the specific test results are detailed in Table 1.
Example 7
The embodiment provides a calcination treatment method of phosphogypsum, which comprises the following steps of (1) mixing phosphogypsum containing phosphorus and fluorine with an additive for 5min to obtain a mixture; wherein the additive amount is 8% of the phosphorus and fluorine-containing phosphogypsum by mass; the additive is ammonium bicarbonate; the mixing manner comprises ball milling;
(2) calcining the mixture obtained in the step (1) at 210 ℃ for 10 hours to obtain a phosphogypsum product;
and (3) carrying out soluble phosphorus and fluorine tests on the obtained phosphogypsum product, wherein the specific test process refers to GB/T23456-2018 phosphogypsum, and the specific test results are detailed in Table 1.
Example 8
The embodiment provides a calcination treatment method of phosphogypsum, which comprises the following steps of (1) mixing phosphogypsum containing phosphorus and fluorine with an additive for 5min to obtain a mixture; wherein the additive amount is 6% of the phosphorus and fluorine-containing phosphogypsum by mass; the additive is ammonium carbonate; the mixing mode comprises crushing;
(2) calcining the mixture obtained in the step (1) at 180 ℃ for 7 hours to obtain a phosphogypsum product;
and (3) carrying out soluble phosphorus and fluorine tests on the obtained phosphogypsum product, wherein the specific test process refers to GB/T23456-2018 phosphogypsum, and the specific test results are detailed in Table 1.
Comparative example 1
The difference from the example 2 is that no additive is added, the obtained phosphogypsum product is tested for soluble phosphorus and fluorine, the specific test process is carried out by referring to GB/T23456-2018 phosphogypsum, and the specific test result is detailed in the table 1.
The phosphogypsum raw material in the embodiment and the comparative example of the invention is phosphogypsum stockpiled in a chemical plant of cupling of Anhui province, the color is grey black, and the pH value is 3.24.
Table 1 test results of phosphogypsum products obtained from comparative example check
| Soluble phosphorus (as P)2O5Calculated)/ | Soluble fluorine/%) | pH | |
| Phosphogypsum raw material | 0.28 | 0.4 | 3.24 |
| Example 1 | 0.07 | 0.05 | 5.64 |
| Example 2 | 0.03 | 0.06 | 6.62 |
| Example 3 | 0.07 | 0.09 | 6.02 |
| Example 4 | 0.06 | 0.07 | 5.04 |
| Example 5 | 0.06 | 0.04 | 5.21 |
| Example 6 | 0.03 | 0.02 | 5.67 |
| Example 7 | 0.03 | 0.07 | 6.04 |
| Example 8 | 0.03 | 0.05 | 6.65 |
| Comparative example 1 | 0.44 | 0.16 | 3.60 |
From the results of the above examples and comparative examples, it can be seen that the method provided by the invention realizes rapid inertization and removal of phosphorus and fluorine in phosphogypsum at a lower temperature by adding additives into phosphogypsum containing phosphorus and fluorine and calcining at a low temperature, and can obtain a phosphogypsum product meeting the first-class requirements in the GB/T23456-2018 specification, and further can be directly used for preparing calcined phosphogypsum.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The calcination treatment method of the phosphogypsum is characterized by comprising the following steps:
(1) mixing phosphorus-and fluorine-containing phosphogypsum with an additive to obtain a mixture;
(2) and (3) calcining the mixture obtained in the step (1) to obtain a phosphogypsum product.
2. The calcination treatment process of claim 1, wherein the additive of step (1) is added in an amount of 0.5 to 10% by mass of the phosphorus and fluorine-containing phosphogypsum.
3. The calcination treatment method according to claim 1 or 2, wherein the additive of step (1) includes 1 or a combination of at least 2 of ammonium chloride, ammonium carbonate, ammonium bicarbonate, ammonium acetate, calcium chloride, calcium acetate, or sodium acetate.
4. The calcination treatment according to any one of claims 1 to 3, wherein the mixing in step (1) includes pulverization and/or ball milling.
5. The calcination treatment method according to any one of claims 1 to 4, wherein the mixing time in the step (1) is 2 to 10 min.
6. The calcination treatment method according to any one of claims 1 to 5, wherein the calcination treatment temperature in the step (2) is 140 to 210 ℃.
7. The calcination treatment according to any one of claims 1 to 6, wherein the calcination treatment in the step (2) is carried out for a time of 3 to 10 hours.
8. The calcination treatment method according to any one of claims 1 to 7, wherein the mixture of step (1) is subjected to sieving;
preferably, the sieve has a mesh size of 100 mesh;
preferably, the sieved undersize product is used for the calcination treatment of step (2).
9. The calcination treatment according to any one of claims 1 to 8, wherein the calcination treatment comprises the steps of:
(1) mixing phosphorus-and fluorine-containing phosphogypsum with an additive for 2-10min to obtain a mixture; wherein the additive amount is 0.5-10% of the phosphorus and fluorine-containing phosphogypsum by mass; the additive comprises 1 or a combination of at least 2 of ammonium chloride, ammonium carbonate, ammonium bicarbonate, ammonium acetate, calcium chloride, calcium acetate, or sodium acetate; the mixing mode comprises crushing and/or ball milling;
(2) calcining the mixture obtained in the step (1) at 140-210 ℃ for 3-10h to obtain a phosphogypsum product;
screening the mixture obtained in the step (1); the size of the screened sieve pore is 100 meshes;
the sieved undersize product is used for the calcination treatment of step (2).
10. Use of the phosphogypsum product obtained from the calcination treatment process according to any one of claims 1 to 9, in the preparation of calcined phosphogypsum.
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