CN114906868B - Phosphogypsum efficient purification method and application - Google Patents
Phosphogypsum efficient purification method and application Download PDFInfo
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- CN114906868B CN114906868B CN202210625383.6A CN202210625383A CN114906868B CN 114906868 B CN114906868 B CN 114906868B CN 202210625383 A CN202210625383 A CN 202210625383A CN 114906868 B CN114906868 B CN 114906868B
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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
- C01F11/46—Sulfates
- C01F11/468—Purification of calcium sulfates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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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
Abstract
The invention relates to the technical field of phosphogypsum modification and application, in particular to a method for efficiently purifying phosphogypsum and application, comprising the following steps: dissolving industrial byproduct phosphogypsum dihydrate in water, sequentially adding a cosolvent, a regulator, a stabilizer, an adsorbent and a foaming agent, uniformly mixing, adding a grinding medium for grinding, and carrying out slurry precipitation, screening, washing and separation after grinding is finished to obtain impurity-removed phosphogypsum slurry; and uniformly mixing the prepared phosphogypsum slurry with the modifier and the crystal form regulator, adding a grinding medium again for wet grinding, and separating and drying after grinding to obtain purified phosphogypsum powder. The invention can not only remarkably solve the problem of phosphogypsum waste, but also improve the purity of phosphogypsum and the application value of phosphogypsum through the combined action of a liquid phase grinding process and chemical physical adsorption. The modified asphalt reduces the mixing temperature of the asphalt, improves the ageing resistance and mechanical property of the asphalt, and prolongs the service life of the asphalt.
Description
Technical Field
The invention relates to the technical field of phosphogypsum modification and application, in particular to a method for efficiently purifying phosphogypsum and application thereof.
Background
Phosphogypsum is waste residue generated in the production process of phosphoric acid and phosphate fertilizer industry, wherein the discharge of the phosphogypsum is about 4-6 tons per ton of phosphoric acid produced, and the discharge of the phosphogypsum residue is about 2 hundred million tons per year worldwide at present, and the annual discharge of China is more than 5000 ten thousand tons. After the phosphogypsum is discharged or piled up and leached by rainwater, fluorine and phosphorus in the phosphogypsum are leached out along with the rainwater and enter soil or rivers to pollute surface water and underground water. Phosphogypsum has become a world problem severely restricting sustainable development and environmental protection in the phosphorus chemical industry.
The main component of phosphogypsum is calcium sulfate dihydrate, which contains a small amount of non-decomposed phosphorite and various impurities such as non-removed phosphoric acid, calcium fluoride, iron and the like. The impurities have a certain influence on the recycling of phosphogypsum, so the pretreatment of phosphogypsum is an important link, and the harmful influence of the impurities can be eliminated or weakened through the pretreatment.
The modified asphalt is asphalt mixture with improved asphalt performance through adding rubber, resin, polymer, waste rubber powder and other modifier or through mild oxidizing treatment. The road surface paved by the said material has good durability and antiwear performance, and it can be used to realize no softening at high temperature and no cracking at low temperature. The inorganic powder modified asphalt has important significance.
Road asphalt is in long-term contact with air during production, and a series of physical and chemical changes such as evaporation, dehydrogenation, oxidation, condensation and the like can occur. At this time, the physical properties of the asphalt are gradually hardened and become brittle, and the asphalt is extremely easy to crack and break under the action of external force, and the original functions of adhesion, sealing and the like cannot be continuously exerted. And the road asphalt is affected by the external environment, so that the internal structure and chemical properties can be irreversibly changed. Inorganic powder modified asphalt
Patent CN202110817401.6 discloses an phosphogypsum asphalt mixture and a preparation method thereof, and the invention realizes the recycling of phosphogypsum resources by applying industrial waste phosphogypsum to the asphalt mixture, reduces environmental pollution and improves the performance of pavement asphalt. However, the phosphogypsum is not purified and decontaminated, and the quality of the phosphogypsum is not improved, so that the asphalt performance of the pavement is not improved, and the risk of impurity leakage exists.
Patent CN201610569842.8 discloses a method for deeply purifying phosphogypsum, which can remarkably improve the whiteness of the phosphogypsum and reduce the contents of impurities such as phosphorus, fluorine, silicon, metal oxide and the like in the phosphogypsum. However, the preparation process is complex, and the concentration of each substance in the reaction system is not well controlled. The energy consumption is large and the environment is not protected.
Disclosure of Invention
The invention aims to provide the high-efficiency phosphogypsum purification method, which not only can remarkably solve the waste problem of phosphogypsum, but also can greatly improve the purity of phosphogypsum through the combined action of a liquid phase grinding process and chemical physical adsorption, optimize organic and inorganic impurities in phosphogypsum, improve the application value of phosphogypsum, and has simple process and easy adjustment.
The second purpose of the invention is to provide an application of phosphogypsum in efficient purification, wherein the high-purity phosphogypsum is used for modifying asphalt, so that the ageing resistance and mechanical property of the asphalt are greatly improved. Meanwhile, the potential hazard of the modified asphalt material is reduced, and the modified asphalt material has great environmental protection value.
The scheme adopted by the invention for achieving one of the purposes is as follows: a method for efficiently purifying phosphogypsum comprises the following steps:
(1) Dissolving 60-80 parts by weight of industrial byproduct phosphogypsum (the main component is calcium sulfate, the content of which is more than 90%) in 100 parts by weight of water, then sequentially adding 3-5 parts by weight of a cosolvent, 1-3 parts by weight of a regulator, 1-3 parts by weight of a stabilizer, 30-40 parts by weight of an adsorbent and 1-4 parts by weight of a foaming agent, uniformly mixing, adding a grinding medium for grinding, and carrying out slurry precipitation, screening, washing and separation after grinding is finished to obtain impurity-removed phosphogypsum slurry;
(2) Uniformly mixing the phosphogypsum slurry prepared in the step (1) with 1-4 parts by weight of modifier and 1-4 parts by weight of crystal form regulator, adding grinding medium again for wet grinding, and separating and drying after grinding is finished to obtain purified phosphogypsum powder.
Preferably, in the step (1), the solvent is at least one of acetic acid, sulfuric acid and citric acid.
Preferably, in the step (1), the regulator is ethylenediamine tetraacetic acid or polyethylene glycol; the stabilizer is any one of octyl phenol polyoxyethylene ether, nonylphenol polyoxyethylene ether and laurinol polyoxyethylene ether.
Preferably, in the step (1), the adsorbent is activated alumina or polyacrylamide.
Preferably, in the step (1), the foaming agent is any one of sodium dodecyl sulfate, sodium alpha-alkenyl sulfonate and sodium fatty alcohol polyoxyethylene ether sulfate.
Preferably, in the step (2), the modifier is sodium sulfate or silica fume; the crystal form regulator is maleic acid or diethyl glycol.
Preferably, in the steps (1) and (2), the grinding medium is zirconia balls or agate balls.
The scheme adopted by the invention for achieving the second purpose is as follows: use of phosphogypsum purified by the method according to any one of claims 1 to 7, characterized in that: and preparing the modified asphalt by adopting the phosphogypsum.
Preferably, the specific preparation method comprises the following steps: heating 100 parts by weight of matrix asphalt to 150-170 ℃, adding 10-15 parts by weight of phosphogypsum powder, adding 5-10 parts by weight of biological oil and 5-10 parts by weight of plasticizer, uniformly stirring and mixing, and swelling and developing at 130-140 ℃ to obtain phosphogypsum modified asphalt.
Preferably, the plasticizer is dioctyl phthalate or dioctyl adipate.
The invention has the following advantages and beneficial effects:
the high-efficiency phosphogypsum purification method can not only remarkably solve the waste problem of phosphogypsum, but also greatly improve the purity of phosphogypsum through the combined action of a liquid-phase grinding process and chemical physical adsorption, optimize organic and inorganic impurities in phosphogypsum, improve the application value of phosphogypsum, and have simple process and easy adjustment.
The high-efficiency phosphogypsum purification method effectively removes impurities such as phosphorus, fluorine, organic matters and the like in the industrial byproduct phosphogypsum dihydrate by a chemical treatment method.
The method for efficiently purifying phosphogypsum reduces the particle size of phosphogypsum, increases the surface area of phosphogypsum in chemical action and improves the purification efficiency through a liquid phase ball milling process.
According to the invention, the asphalt is modified by the high-purity phosphogypsum, the mixing temperature of the asphalt is reduced to a certain extent, and the ageing resistance and mechanical property of the asphalt can be effectively improved, so that the service life of the asphalt is prolonged. Meanwhile, the potential hazard of the modified asphalt material is reduced, and the modified asphalt material has great environmental protection value. The asphalt material widens the application field of asphalt and provides a good material selection for asphalt roads and asphalt coiled materials.
Detailed Description
For a better understanding of the present invention, the following examples are further illustrative of the present invention, but the contents of the present invention are not limited to the following examples only.
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The invention will be further illustrated, but is not limited, by the following examples.
Example 1
A method for efficiently purifying phosphogypsum and modifying asphalt thereof comprises the following steps: (1) 60 parts by weight of industrial byproduct phosphogypsum (the main component is calcium sulfate, the content is more than 90%) is dissolved in 100 parts by weight of water, then 3 parts by weight of a cosolvent, 1 part by weight of a regulator, 1 part by weight of a stabilizer, 30 parts by weight of an adsorbent and 1 part by weight of a foaming agent are sequentially added to be uniformly mixed, a grinding medium is added at normal temperature, and the mixture is transferred to a stirring tank for grinding, and after grinding for 40 minutes, slurry precipitation, screening, washing and separation are carried out, so that the impurity-removed phosphogypsum slurry is obtained.
(2) Uniformly mixing the phosphogypsum slurry, 1 part by weight of modifier and 1 part by weight of crystal form regulator, adding a grinding medium again for wet grinding, further optimizing after grinding for 30min, separating and drying to obtain modified phosphogypsum powder.
(3) Preheating 100 parts by weight of matrix asphalt in an oven for 30min, transferring to an oil bath, heating to 150 ℃, adding 10 parts by weight of phosphogypsum powder, adding 5 parts by weight of biological oil, simultaneously adding 5 parts by weight of plasticizer, stirring for 60min at 3000r/min by a high-speed shearing machine, and finally placing the asphalt in an oven at 135 ℃ to swell and develop for 20min, thereby obtaining phosphogypsum modified asphalt.
Example 2
A method for efficiently purifying phosphogypsum and modifying asphalt thereof comprises the following steps: (1) Dissolving 65 parts by weight of industrial byproduct phosphogypsum (the main component is calcium sulfate, the content of which is more than 90%) in 100 parts by weight of water, then sequentially adding 3 parts by weight of a cosolvent, 1 part by weight of a regulator, 1 part by weight of a stabilizer, 30 parts by weight of an adsorbent and 2 parts by weight of a foaming agent, uniformly mixing, adding a grinding medium at normal temperature, transferring to a stirring tank for grinding, and carrying out slurry precipitation, screening, washing and separation after grinding for 50 minutes to obtain the impurity-removed phosphogypsum slurry.
(2) Uniformly mixing the phosphogypsum slurry with 2 parts by weight of modifier and 2 parts by weight of crystal form regulator, adding a grinding medium again for wet grinding, further optimizing after grinding for 40min, separating and drying to obtain modified phosphogypsum powder.
(3) Preheating 100 parts by weight of matrix asphalt in an oven for 35min, transferring to an oil bath, heating to 155 ℃, adding 11 parts by weight of phosphogypsum powder, adding 6 parts by weight of biological oil, simultaneously adding 6 parts by weight of plasticizer, stirring for 70min at 3500r/min by a high-speed shearing machine, and finally placing the asphalt in an oven at 135 ℃ to swell and develop for 20min, thereby obtaining phosphogypsum modified asphalt.
Example 3
A method for efficiently purifying phosphogypsum and modifying asphalt thereof comprises the following steps: (1) 70 parts by weight of industrial byproduct phosphogypsum (the main component is calcium sulfate, the content is more than 90%) is dissolved in 100 parts by weight of water, then 4 parts by weight of a cosolvent, 1 part by weight of a regulator, 1 part by weight of a stabilizer, 35 parts by weight of an adsorbent and 2 parts by weight of a foaming agent are sequentially added to be uniformly mixed, a grinding medium is added at normal temperature, and the mixture is transferred to a stirring tank for grinding, and after grinding for 60 minutes, slurry precipitation, screening, washing and separation are carried out, so that the impurity-removed phosphogypsum slurry is obtained.
(2) Uniformly mixing the phosphogypsum slurry with 2 parts by weight of modifier and 2 parts by weight of crystal form regulator, adding a grinding medium again for wet grinding, further optimizing after grinding for 50min, separating and drying to obtain modified phosphogypsum powder.
(3) Preheating 100 parts by weight of matrix asphalt in an oven for 40min, transferring to an oil bath, heating to 160 ℃, adding 12 parts by weight of phosphogypsum powder, adding 7 parts by weight of bio-oil, simultaneously adding 7 parts by weight of plasticizer, stirring for 80min at 4000r/min by adopting a high-speed shearing machine, and finally placing the asphalt in an oven at 135 ℃ to swell and develop for 20min, thereby obtaining phosphogypsum modified asphalt.
Example 4
A method for efficiently purifying phosphogypsum and modifying asphalt thereof comprises the following steps: (1) 75 parts by weight of industrial byproduct phosphogypsum (the main component is calcium sulfate, the content is more than 90%) is dissolved in 100 parts by weight of water, then 4 parts by weight of a cosolvent, 2 parts by weight of a regulator, 2 parts by weight of a stabilizer, 35 parts by weight of an adsorbent and 3 parts by weight of a foaming agent are sequentially added to be uniformly mixed, a grinding medium is added at normal temperature, and the mixture is transferred to a stirring tank for grinding, and after grinding for 80 minutes, slurry precipitation, screening, washing and separation are carried out, so that the impurity-removed phosphogypsum slurry is obtained.
(2) Uniformly mixing the phosphogypsum slurry, 3 parts by weight of modifier and 3 parts by weight of crystal form regulator, adding a grinding medium again for wet grinding, further optimizing after grinding for 50min, separating and drying to obtain modified phosphogypsum powder.
(3) Preheating 100 parts by weight of matrix asphalt in an oven for 40min, transferring to an oil bath, heating to 165 ℃, adding 13 parts by weight of phosphogypsum powder, adding 8 parts by weight of biological oil, simultaneously adding 8 parts by weight of plasticizer, stirring for 80min at 4500r/min by a high-speed shearing machine, and finally placing the asphalt in an oven at 135 ℃ for swelling and developing for 20min, thereby obtaining phosphogypsum modified asphalt.
Example 5
A method for efficiently purifying phosphogypsum and modifying asphalt thereof comprises the following steps: (1) 80 parts by weight of industrial byproduct phosphogypsum (the main component is calcium sulfate, the content is more than 90%) is dissolved in 100 parts by weight of water, then 5 parts by weight of a cosolvent, 3 parts by weight of a regulator, 3 parts by weight of a stabilizer, 35 parts by weight of an adsorbent and 3 parts by weight of a foaming agent are sequentially added to be uniformly mixed, a grinding medium is added at normal temperature, and the mixture is transferred to a stirring tank for grinding, and after grinding for 90 minutes, slurry precipitation, screening, washing and separation are carried out, so that the impurity-removed phosphogypsum slurry is obtained.
(2) Uniformly mixing the phosphogypsum slurry, 3 parts by weight of modifier and 4 parts by weight of crystal form regulator, adding a grinding medium again for wet grinding, further optimizing after grinding for 60min, separating and drying to obtain modified phosphogypsum powder.
(3) Preheating 100 parts by weight of matrix asphalt in an oven for 45min, transferring to an oil bath, heating to 165 ℃, adding 14 parts by weight of phosphogypsum powder, adding 9 parts by weight of biological oil, simultaneously adding 9 parts by weight of plasticizer, stirring for 90min at 4500r/min by a high-speed shearing machine, and finally placing the asphalt in an oven at 135 ℃ for swelling and developing for 20min, thereby obtaining phosphogypsum modified asphalt.
Example 6
A method for efficiently purifying phosphogypsum and modifying asphalt thereof comprises the following steps: (1) 80 parts by weight of industrial byproduct phosphogypsum (the main component is calcium sulfate, the content is more than 90%) is dissolved in 100 parts by weight of water, then 5 parts by weight of a cosolvent, 3 parts by weight of a regulator, 3 parts by weight of a stabilizer, 40 parts by weight of an adsorbent and 4 parts by weight of a foaming agent are sequentially added to be uniformly mixed, a grinding medium is added at normal temperature, and the mixture is transferred to a stirring tank for grinding, and after grinding for 90 minutes, slurry precipitation, screening, washing and separation are carried out, so that the impurity-removed phosphogypsum slurry is obtained.
(2) Uniformly mixing the phosphogypsum slurry, 4 parts by weight of modifier and 4 parts by weight of crystal form regulator, adding a grinding medium again for wet grinding, further optimizing after grinding for 60min, separating and drying to obtain modified phosphogypsum powder.
(3) And (3) preheating 100 parts by weight of matrix asphalt in an oven for 45min, transferring to an oil bath, heating to 170 ℃, adding 15 parts by weight of phosphogypsum powder, adding 10 parts by weight of biological oil, simultaneously adding 10 parts by weight of plasticizer, stirring for 90min at 5000r/min by a high-speed shearing machine, and finally placing the asphalt in an oven at 135 ℃ to swell and develop for 20min, thereby obtaining phosphogypsum modified asphalt.
The phosphogypsum materials prepared in examples 1 to 6 have the following data in Table 1:
TABLE 1
The basic properties of the modified asphalt prepared in examples 1 to 6 were compared with that of a commercially available 70# base asphalt, and the results are shown in Table 2 below:
TABLE 2
As can be seen from the data in Table 1, the phosphogypsum materials prepared in examples 1 to 6 of the present invention have the impurity content reduced from 27.5% to 1.7% by the combined action of the chemical treatment and the ball milling process, and the impurity removal effect is remarkable. The phosphogypsum powder prepared in examples 1 to 6 has a purity of 98.3% in example 5, which shows that the chemical treatment effect is increased with the increase of the wet milling process time, and the reaction is more complete, so that the purity of the product is higher.
As can be seen from the data in Table 2, the modified asphalt prepared in examples 1 to 6 of the invention has penetration from 74.2 ℃ to 65.9 ℃, which shows that the hardness of the asphalt is reduced, the softening point is increased from 50.8 ℃ to 62.2 ℃, which shows that the high temperature resistance is improved to a certain extent, and the aging 5h residual penetration ratio data of the film oven shows that the aging 5h residual penetration ratio of the modified low-carbon asphalt prepared in examples 1 to 6 is 11.2 to 31.5%, which shows that the modified asphalt has good aging resistance effect.
While the invention has been described with respect to the preferred embodiments, it will be understood that the invention is not limited thereto, but is capable of modification and variation without departing from the spirit of the invention, as will be apparent to those skilled in the art.
Claims (6)
1. The high-efficiency phosphogypsum purification method is characterized by comprising the following steps of:
(1) Dissolving 60-80 parts by weight of industrial byproduct phosphogypsum in 100 parts by weight of water, sequentially adding 3-5 parts by weight of a cosolvent, 1-3 parts by weight of a regulator, 1-3 parts by weight of a stabilizer, 30-40 parts by weight of an adsorbent and 1-4 parts by weight of a foaming agent, uniformly mixing, adding a grinding medium for grinding, and carrying out slurry precipitation, screening, washing and separation after grinding is finished to obtain the impurity-removed phosphogypsum slurry;
(2) Uniformly mixing the phosphogypsum slurry prepared in the step (1) with 1-4 parts by weight of modifier and 1-4 parts by weight of crystal form regulator, adding grinding medium again for wet grinding, and separating and drying after grinding to obtain purified phosphogypsum powder;
in the step (1), the cosolvent is at least one of acetic acid, sulfuric acid and citric acid; the regulator is ethylenediamine tetraacetic acid or polyethylene glycol; the stabilizer is any one of octyl phenol polyoxyethylene ether, nonylphenol polyoxyethylene ether and laurinol polyoxyethylene ether; the foaming agent is any one of sodium dodecyl sulfate, alpha-alkenyl sodium sulfonate and fatty alcohol polyoxyethylene ether sodium sulfate;
in the step (2), the modifier is sodium sulfate or silica fume powder; the crystal form regulator is maleic acid or diethyl glycol.
2. The method for high-efficiency purification of phosphogypsum according to claim 1, which is characterized in that: in the step (1), the adsorbent is activated alumina or polyacrylamide.
3. The method for high-efficiency purification of phosphogypsum according to claim 1, which is characterized in that: in the steps (1) and (2), the grinding medium is zirconia balls or agate balls.
4. Use of phosphogypsum purified by the method according to any one of claims 1 to 3, characterized in that: and preparing the modified asphalt by adopting the phosphogypsum.
5. The use according to claim 4, characterized in that: the specific preparation method comprises the following steps: heating 100 parts by weight of matrix asphalt to 150-170 ℃, adding 10-15 parts by weight of phosphogypsum powder, adding 5-10 parts by weight of biological oil and 5-10 parts by weight of plasticizer, uniformly stirring and mixing, and swelling and developing at 130-140 ℃ to obtain phosphogypsum modified asphalt.
6. The use according to claim 5, characterized in that: the plasticizer is dioctyl phthalate or dioctyl adipate.
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