CN108862337B - Method for preparing high-purity magnesium oxide by pyrolyzing magnesium sulfate - Google Patents
Method for preparing high-purity magnesium oxide by pyrolyzing magnesium sulfate Download PDFInfo
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- CN108862337B CN108862337B CN201810951474.2A CN201810951474A CN108862337B CN 108862337 B CN108862337 B CN 108862337B CN 201810951474 A CN201810951474 A CN 201810951474A CN 108862337 B CN108862337 B CN 108862337B
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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
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
- C01F5/12—Magnesia by thermal decomposition of magnesium compounds by thermal decomposition of magnesium sulfate, with or without reduction
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- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The method for preparing high-purity magnesium oxide by pyrolyzing magnesium sulfate comprises the following steps: mixing a P204 extracting agent with the light calcined powder slurry to prepare P204 magnesium soap; extracting the high-magnesium wastewater by using P204 magnesium soap to obtain magnesium sulfate raffinate; sequentially carrying out oil removal and evaporation concentration on the magnesium sulfate raffinate to obtain magnesium sulfate heptahydrate crystals; sequentially calcining and grinding the magnesium sulfate heptahydrate crystal to obtain anhydrous magnesium sulfate powder; mixing anhydrous magnesium sulfate powder and petroleum coke powder, and then carrying out pyrolysis to obtain high-purity magnesium oxide. The raw materials of the invention are petroleum coke and high-magnesium wastewater, the high-magnesium wastewater not only has wide sources, but also can effectively recycle resources, and the petroleum coke has low cost and is easy to obtain; the purity of the obtained high-purity magnesium oxide as a target product is more than 99.5 percent, and can reach or even exceed the purity of the high-purity magnesium oxide obtained by the existing method.
Description
Technical Field
The invention belongs to the field of metallurgy, and particularly relates to a method for preparing high-purity magnesium oxide by pyrolyzing magnesium sulfate.
Background
Magnesium oxide is used as a chemical raw material with wide application, and plays an important role in the fields of metallurgy chemical industry, food, medicine, agriculture and the like. The current methods for preparing magnesium oxide by using magnesium sulfate generally comprise two methods: the method is a precipitation method, namely magnesium sulfate and magnesium hydroxide are used as raw materials to prepare high-purity magnesium oxide through high-temperature calcination, the purity of the magnesium oxide prepared by the method can reach 99%, but the method uses sodium hydroxide as a precipitator, so that the production cost is increased, and the reaction conditions are not easy to control; the other method is to prepare magnesium oxide by magnesium sulfate pyrolysis, namely, magnesium sulfate is reduced by a solid reducing agent to prepare magnesium oxide, and the common solid reducing agent is coal, natural gas and the like. The invention patent with publication number CN102173439B discloses a method for preparing high-purity magnesium oxide by reducing and pyrolyzing magnesium sulfate with natural gas, but the method requires that the purity of magnesium sulfate raw material is more than 99%, and the cost of natural gas is higher.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing high-purity magnesium oxide by using high-magnesium wastewater and petroleum coke powder generated in the production process as raw materials, and the method has the advantages of low production cost, less environmental pollution and high purity of the obtained high-purity magnesium oxide product.
The invention adopts the following technical scheme:
the method for preparing high-purity magnesium oxide by pyrolyzing magnesium sulfate is characterized by comprising the following steps of:
(1) mixing a P204 extracting agent with the light calcined powder slurry to prepare P204 magnesium soap;
(2) extracting the high-magnesium wastewater by using the P204 magnesium soap in the step (1) to obtain magnesium sulfate raffinate;
(3) sequentially carrying out oil removal and evaporation concentration on the magnesium sulfate raffinate in the step (2) to obtain magnesium sulfate heptahydrate crystals;
(4) sequentially calcining and grinding the magnesium sulfate heptahydrate crystals in the step (3) to obtain anhydrous magnesium sulfate powder;
(5) and (4) mixing the anhydrous magnesium sulfate powder and the petroleum coke powder in the step (4) and then carrying out pyrolysis to obtain the high-purity magnesium oxide.
The method is characterized in that in the step (1), the P204 extractant is a mixture of P204 and solvent oil, and the volume ratio of the P204 to the solvent oil is 1: 3-9; the mass percentage concentration of the light calcined powder in the light calcined powder slurry is 10-50 percent; the mass ratio of the P204 extractant to MgO contained in the light calcined powder slurry is 80-800:1, and the saponification rate of the P204 magnesium soap is controlled to be 10-70%.
The method is characterized in that the pH value of the P204 magnesium soap extracted from the high-magnesium wastewater in the step (2) is 2.5-6.5, and the volume ratio of the P204 magnesium soap to the high-magnesium wastewater is 1-5: 1.
The method is characterized in that the components and the concentrations of the high-magnesium wastewater in the step (2) are as follows: 20g/L-50g/L magnesium, 0.1g/L-0.6g/L calcium, less than 1mg/L nickel, less than 1mg/L cobalt and less than 1mg/L manganese; the magnesium sulfate raffinate comprises the following components in concentration: 20g/L-50g/L of magnesium, less than 0.1g/L of calcium, less than 1mg/L of nickel, less than 1mg/L of cobalt and less than 1mg/L of manganese.
The method is characterized in that the calcining temperature in the step (4) is 200-500 ℃, and the calcining time is 60-360 min; the particle size of the anhydrous magnesium sulfate powder is 100-500 meshes.
The method as described above, wherein the petroleum coke powder in the step (5) has a particle size of 50 mesh to 500 mesh.
The method is characterized in that in the step (5), the mass ratio of the anhydrous magnesium sulfate powder to the petroleum coke powder is 3-7:1, the temperature for pyrolysis after mixing is 800-1100 ℃, and the time for pyrolysis after mixing is 40-120 min.
The invention has the beneficial effects that: compared with the existing method for producing high-purity magnesium oxide, the raw materials of the method are petroleum coke and high-magnesium wastewater generated in the production process, the high-magnesium wastewater not only has wide sources, but also can effectively recover resources, and the petroleum coke has lower cost and is easier to obtain compared with the raw materials such as natural gas used in the existing method; the purity of the target product high-purity magnesium oxide obtained by the method is more than 99.5 percent, and can reach or even exceed the purity of the high-purity magnesium oxide obtained by the existing method.
Drawings
FIG. 1 is a schematic process flow diagram of the process of the present invention.
Detailed Description
The method for preparing high-purity magnesium oxide by pyrolyzing magnesium sulfate comprises the following steps: (1) mixing a P204 extracting agent with the light calcined powder slurry to prepare P204 magnesium soap; the P204 extractant is a mixture of P204 and solvent oil, and the volume ratio of the P204 to the solvent oil is 1: 3-9; the mass percentage concentration of the light calcined powder in the light calcined powder slurry is 10-50 percent; the mass ratio of the P204 extractant to MgO contained in the light calcined powder slurry is 80-800:1, and the saponification rate of the P204 magnesium soap is controlled to be 10-70%. (2) Extracting the high-magnesium wastewater by using the P204 magnesium soap in the step (1) to obtain magnesium sulfate raffinate; the pH value of the P204 magnesium soap for extracting the high-magnesium wastewater is 2.5-6.5, and the volume ratio of the P204 magnesium soap to the high-magnesium wastewater is 1-5: 1; the high-magnesium wastewater comprises the following components in percentage by weight: 20g/L-50g/L magnesium, 0.1g/L-0.6g/L calcium, less than 1mg/L nickel, less than 1mg/L cobalt and less than 1mg/L manganese; the magnesium sulfate raffinate comprises the following components in concentration: 20g/L-50g/L of magnesium, less than 0.1g/L of calcium, less than 1mg/L of nickel, less than 1mg/L of cobalt and less than 1mg/L of manganese. (3) Sequentially carrying out oil removal and evaporation concentration on the magnesium sulfate raffinate in the step (2) to obtain magnesium sulfate heptahydrate crystals; (4) sequentially calcining and grinding the magnesium sulfate heptahydrate crystals in the step (3) to obtain anhydrous magnesium sulfate powder; the calcining temperature is 200-500 ℃, and the calcining time is 60-360 min; the particle size of the anhydrous magnesium sulfate powder is 100-500 meshes; the grain size of the petroleum coke powder is 50-500 meshes. (5) Mixing the anhydrous magnesium sulfate powder and the petroleum coke powder in the step (4) and then carrying out pyrolysis to obtain high-purity magnesium oxide; the mass ratio of the anhydrous magnesium sulfate powder to the petroleum coke powder is 3-7:1, the temperature for pyrolysis after mixing is 800-1100 ℃, and the time for pyrolysis after mixing is 40-120 min.
Example 1
100L P204 of an extracting agent is measured, wherein the volume ratio of P204 to solvent oil is 1: 9, weighing 60g of light calcined powder to prepare light calcined powder slurry with the weight percentage concentration of the light calcined powder being 10%, mixing a P204 extracting agent with the light calcined powder slurry to prepare P204 magnesium soap, and controlling the saponification rate of the P204 magnesium soap to be 15%; extracting 100L of high-magnesium wastewater by using P204 magnesium soap to obtain magnesium sulfate raffinate, wherein the extracted pH is 2.5, and the high-magnesium wastewater comprises the following components in percentage by weight: 22g/L of magnesium, 0.55g/L of calcium, 0.6mg/L of nickel, 0.6mg/L of cobalt and 0.6mg/L of manganese, wherein the magnesium sulfate raffinate comprises the following components in percentage by weight: 21.9g/L of magnesium, 0.08g/L of calcium, 0.6mg/L of nickel, 0.6mg/L of cobalt and 0.6mg/L of manganese; sequentially carrying out oil removal and evaporation concentration on the magnesium sulfate raffinate to obtain 22.3kg of magnesium sulfate heptahydrate crystals; calcining 22.3kg of magnesium sulfate heptahydrate crystals at 250 ℃ for 360min to obtain 10.9kg of anhydrous magnesium sulfate, and grinding to obtain 500-mesh anhydrous magnesium sulfate powder; mixing 10.9kg of anhydrous magnesium sulfate powder and 1.7kg of petroleum coke powder with the grain size of about 500 meshes, then carrying out pyrolysis to obtain 3.6kg of product, wherein the pyrolysis temperature is 1100 ℃, the pyrolysis time is 45min, and tail gas is absorbed by a tail gas absorption treatment device. The purity of the high-purity magnesium oxide in the product is 99.8%.
Example 2
100L P204 of an extracting agent is measured, wherein the volume ratio of P204 to solvent oil is 1: weighing 420g of light calcined powder to prepare light calcined powder slurry with the weight percentage concentration of 20% of the light calcined powder, and mixing a P204 extracting agent and the light calcined powder slurry to prepare P204 magnesium soap, wherein the saponification rate of the P204 magnesium soap is controlled to be 35%; extracting 50L of high-magnesium wastewater by using P204 magnesium soap to obtain magnesium sulfate raffinate, wherein the extracted pH is 3, and the high-magnesium wastewater comprises the following components in percentage by weight: 25g/L of magnesium, 0.5g/L of calcium, 0.5mg/L of nickel, 0.6mg/L of cobalt and 0.5mg/L of manganese, wherein the magnesium sulfate raffinate comprises the following components in percentage by weight: 24.5g/L of magnesium, 0.05g/L of calcium, 0.5mg/L of nickel, 0.6mg/L of cobalt and 0.5mg/L of manganese; sequentially carrying out oil removal and evaporation concentration on the magnesium sulfate raffinate to obtain 12.5kg of magnesium sulfate heptahydrate crystals; calcining 22.3kg of magnesium sulfate heptahydrate crystals at 480 ℃ for 90min to obtain 6.1kg of anhydrous magnesium sulfate, and grinding to obtain 100-mesh anhydrous magnesium sulfate powder; mixing 6.1kg of anhydrous magnesium sulfate powder and 2kg of petroleum coke powder with the grain size of about 50 meshes, then carrying out pyrolysis to obtain 2kg of product, wherein the pyrolysis temperature is 850 ℃, the pyrolysis time is 120min, and tail gas is absorbed and treated by a tail gas absorption and treatment device. The purity of the high-purity magnesium oxide in the product is 99.8%.
Example 3
100L P204 of an extracting agent is measured, wherein the volume ratio of P204 to solvent oil is 1: 5.7, weighing 180g of light calcined powder to prepare light calcined powder slurry with the light calcined powder mass percentage concentration of 30%, and mixing a P204 extracting agent and the light calcined powder slurry to prepare the P204 magnesium soap, wherein the saponification rate of the P204 magnesium soap is controlled at 20%; extracting 33L of high-magnesium wastewater by using P204 magnesium soap to obtain magnesium sulfate raffinate, wherein the extracted pH is 2.5, and the high-magnesium wastewater comprises the following components in percentage by weight: 20g/L of magnesium, 0.15g/L of calcium, 0.5mg/L of nickel, 0.5mg/L of cobalt and 0.5mg/L of manganese, wherein the magnesium sulfate raffinate comprises the following components in percentage by weight: 20g/L of magnesium, 0.01g/L of calcium, 0.5mg/L of nickel, 0.5mg/L of cobalt and 0.5mg/L of manganese; sequentially carrying out oil removal and evaporation concentration on the magnesium sulfate raffinate to obtain 6.8kg of magnesium sulfate heptahydrate crystals; calcining 6.8kg of magnesium sulfate heptahydrate crystals at 380 ℃ for 150min to obtain 3.3kg of anhydrous magnesium sulfate, and grinding to obtain 150-mesh anhydrous magnesium sulfate powder; mixing 3.3kg of anhydrous magnesium sulfate powder and 0.7kg of petroleum coke powder with the grain size of about 200 meshes, then carrying out pyrolysis to obtain 1.1kg of product, wherein the pyrolysis temperature is 900 ℃, the pyrolysis time is 90min, and tail gas is absorbed by a tail gas absorption treatment device. The purity of the high-purity magnesium oxide in the product is 99.6%.
Example 4
100L P204 of an extracting agent is measured, wherein the volume ratio of P204 to solvent oil is 1: weighing 720g of light calcined powder to prepare light calcined powder slurry with the weight percentage concentration of the light calcined powder being 50%, mixing a P204 extracting agent with the light calcined powder slurry to prepare P204 magnesium soap, and controlling the saponification rate of the P204 magnesium soap to be 60%; extracting 20L of high-magnesium wastewater by using P204 magnesium soap to obtain magnesium sulfate raffinate, wherein the extracted pH is 5.5, and the high-magnesium wastewater comprises the following components in percentage by weight: 35g/L of magnesium, 0.45g/L of calcium, 0.3mg/L of nickel, 0.3mg/L of cobalt and 0.3mg/L of manganese, wherein the magnesium sulfate raffinate comprises the following components in percentage by weight: 34.5g/L of magnesium, 0.01g/L of calcium, 0.3mg/L of nickel, 0.3mg/L of cobalt and 0.3mg/L of manganese; sequentially carrying out oil removal and evaporation concentration on the magnesium sulfate raffinate to obtain 7.06kg of magnesium sulfate heptahydrate crystals; calcining 7.06kg of magnesium sulfate heptahydrate crystal at 400 ℃ for 120min to obtain 3.4kg of anhydrous magnesium sulfate, and grinding to obtain 250-mesh anhydrous magnesium sulfate powder; mixing 3.4kg of anhydrous magnesium sulfate powder and 0.6kg of petroleum coke powder with the grain size of about 300 meshes, then carrying out pyrolysis to obtain 1.15kg of product, wherein the pyrolysis temperature is 1100 ℃, the pyrolysis time is 50min, and tail gas is absorbed by a tail gas absorption treatment device. The purity of the high-purity magnesium oxide in the product is 99.7%.
Example 5
100L P204 of an extracting agent is measured, wherein the volume ratio of P204 to solvent oil is 1: weighing 1000g of light calcined powder to prepare light calcined powder slurry with the weight percentage concentration of the light calcined powder being 45%, mixing a P204 extracting agent with the light calcined powder slurry to prepare P204 magnesium soap, and controlling the saponification rate of the P204 magnesium soap to be 68%; extracting 25L of high-magnesium wastewater by using P204 magnesium soap to obtain magnesium sulfate raffinate, wherein the extracted pH is 6.5, and the high-magnesium wastewater comprises the following components in percentage by weight: 45g/L of magnesium, 0.5g/L of calcium, 0.3mg/L of nickel, 0.2mg/L of cobalt and 0.1mg/L of manganese, wherein the magnesium sulfate raffinate comprises the following components in percentage by weight: 44.5g/L magnesium, 0.01g/L calcium, 0.3mg/L nickel, 0.2mg/L cobalt and 0.1mg/L manganese; sequentially carrying out oil removal and evaporation concentration on the magnesium sulfate raffinate to obtain 5.5kg of magnesium sulfate heptahydrate crystals; calcining 5.5g of magnesium sulfate heptahydrate crystals at 250 ℃ for 360min to obtain 2.7kg of anhydrous magnesium sulfate, and grinding to obtain 500-mesh anhydrous magnesium sulfate powder; mixing 2.7kg of anhydrous magnesium sulfate powder and 0.4kg of petroleum coke powder with the grain size of about 500 meshes, then carrying out pyrolysis to obtain 0.9kg of product, wherein the pyrolysis temperature is 1000 ℃, the pyrolysis time is 60min, and tail gas is absorbed by a tail gas absorption treatment device. The purity of the high-purity magnesium oxide in the product is 99.8%.
Claims (3)
1. The method for preparing high-purity magnesium oxide by pyrolyzing magnesium sulfate is characterized by comprising the following steps of:
(1) mixing a P204 extracting agent with the light calcined powder slurry to prepare P204 magnesium soap; the P204 extractant is a mixture of P204 and solvent oil, and the volume ratio of the P204 to the solvent oil is 1: 3-9; the mass percentage concentration of the light calcined powder in the light calcined powder slurry is 10-50 percent; the mass ratio of the P204 extractant to MgO contained in the light calcined powder slurry is 80-800:1, and the saponification rate of the P204 magnesium soap is controlled to be 10-70%;
(2) extracting the high-magnesium wastewater by using the P204 magnesium soap in the step (1) to obtain magnesium sulfate raffinate; the pH value of the P204 magnesium soap for extracting the high-magnesium wastewater is 2.5-6.5, and the volume ratio of the P204 magnesium soap to the high-magnesium wastewater is 1-5: 1; the high-magnesium wastewater comprises the following components in percentage by weight: 20g/L-50g/L magnesium, 0.1g/L-0.6g/L calcium, less than 1mg/L nickel, less than 1mg/L cobalt and less than 1mg/L manganese;
(3) sequentially carrying out oil removal and evaporation concentration on the magnesium sulfate raffinate in the step (2) to obtain magnesium sulfate heptahydrate crystals;
(4) sequentially calcining and grinding the magnesium sulfate heptahydrate crystals in the step (3) to obtain anhydrous magnesium sulfate powder; the calcining temperature is 200-500 ℃, and the calcining time is 60-360 min; the particle size of the anhydrous magnesium sulfate powder is 100-500 meshes;
(5) mixing the anhydrous magnesium sulfate powder and the petroleum coke powder in the step (4) and then carrying out pyrolysis to obtain high-purity magnesium oxide; the temperature for pyrolysis after mixing is 800-1100 ℃, and the time for pyrolysis after mixing is 40-120 min.
2. The process according to claim 1, wherein the magnesium sulfate raffinate in step (2) has the following composition and concentration: 20g/L-50g/L of magnesium, less than 0.1g/L of calcium, less than 1mg/L of nickel, less than 1mg/L of cobalt and less than 1mg/L of manganese.
3. The method according to claim 1, wherein the petroleum coke powder in the step (5) has a particle size of 50 mesh to 500 mesh; in the step (5), the mass ratio of the anhydrous magnesium sulfate powder to the petroleum coke powder is 3-7: 1.
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| CN112661178A (en) * | 2020-12-25 | 2021-04-16 | 山东信能达工程科技有限公司 | Preparation and production process of high-purity magnesium oxide |
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