CN115124055A - Low-cost, efficient and environment-friendly production process of light magnesium carbonate and light magnesium oxide - Google Patents
Low-cost, efficient and environment-friendly production process of light magnesium carbonate and light magnesium oxide Download PDFInfo
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- CN115124055A CN115124055A CN202210841019.3A CN202210841019A CN115124055A CN 115124055 A CN115124055 A CN 115124055A CN 202210841019 A CN202210841019 A CN 202210841019A CN 115124055 A CN115124055 A CN 115124055A
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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
- C01F5/24—Magnesium carbonates
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention provides a low-cost, high-efficiency and environment-friendly production process of light magnesium carbonate and light magnesium oxide, which comprises the following steps: s1: crushing, fine grinding and wet deferrization of serpentine to obtain serpentine slurry, carrying out filter pressing, drying, calcining in a calcining furnace, cooling, crushing and then feeding into a hydration tank; s2: the temperature of the hydration tank is more than or equal to 80 ℃, the time is more than or equal to 1h, and the solid-liquid ratio of the hydration slurry is 4: 1, the stirring speed is more than or equal to 150r/min, and the solid-liquid ratio of the hydrated slurry is kept at 10: 1, sending the mixture into an aging pool, standing for 2 hours, and then sending the mixture into a carbonizer; compared with a sulfuric acid method, a hydrochloric acid method and an ammonium salt method, the method does not produce new compounds, thoroughly ensures the purity of the raw materials, can easily obtain high-quality light magnesium carbonate with MgO being more than or equal to 42 percent and high-quality light magnesium oxide with MgO being more than or equal to 98 percent, has the advantages of environmental protection, friendliness, low calcination temperature, short reaction time, mild reaction conditions, high recovery rate and the like, and is suitable for industrial production.
Description
Technical Field
The invention particularly relates to a production process of light magnesium carbonate and light magnesium oxide with low cost, high efficiency and environmental protection.
Background
Light magnesium carbonate is a chemical substance with the molecular formula of xMgCO 3. yMg (OH) 2. z3H 2O. Appearance: white monoclinic crystalline or amorphous powder, non-toxic, tasteless, stable in air. The light magnesium carbonate generally includes pharmaceutical grade magnesium carbonate, food grade magnesium carbonate, analytical pure magnesium carbonate, chemical pure magnesium carbonate, industrial hydrated basic magnesium carbonate, and the like. In recent years, magnesium carbonate enterprises in China actively carry out technical innovation, the magnesium carbonate market is developed rapidly every year, the use amount of light magnesium carbonate in the market is continuously increased in recent years, and the market share of rubber, glass, ceramics, ink and the like is also continuously increased.
The light magnesium carbonate is used as a medical intermediate, an antacid, a drying agent, a color fixative, a carrier and an anticaking agent; can be used as additive and magnesium compensator in food; in fine chemistry for the production of chemical reagents; as reinforcing agent and filler in rubber; can be used as a fireproof heat-insulating material with heat insulation and high temperature resistance; manufacturing a high-grade glass product; the enamel ceramic plays a role in surface brightness; making magnesium salt, pigment, paint, daily cosmetics, shipbuilding and boiler. The coating industry is used as filler for accessory pigments, paints and inks to increase whiteness and hiding power. With the rapid development of fine chemical products, magnesium salt seriation and special products are rapidly developing. From the point of view of performance and use, light magnesium carbonate is one of the largest magnesium salt series products produced and sold at present. With the development of industries such as metallurgy, plastics, rubber, paint, papermaking and the like, the demand of light magnesium carbonate is on the trend of rising year by year.
In recent years, the dosage of the light magnesium carbonate in the domestic market is increased rapidly and is kept to be increased by more than 10 percent all the time, and the price is basically kept stable. At present, the total demand of various magnesium salts in various industries is about 120 ten thousand t each year, wherein the light magnesium carbonate is required to be about 24-45 ten thousand t in the industries of rubber, plastics, paper making and the like, the consumption of ceramic enterprises is more than 12 ten thousand t, and various magnesium salt products are required to be about 45-75 ten thousand t in other industries. Meanwhile, the country still exports a part of magnesium salt products outwards every year, and the export amount of light magnesium carbonate shows a high-speed increasing trend in recent years.
The current domestic method for producing light magnesium carbonate comprises the following steps:
1. magnesite (MgCO3) is mixed with coke and then roasted to obtain magnesium oxide. Adding water into the mixture to form paste, introducing CO2 into the paste to obtain magnesium bicarbonate, filtering the magnesium bicarbonate, and heating the filtrate to obtain basic carbonate precipitate.
2. Heating dolomite (MgCO 3. CaCO3) with slow fire to decompose only magnesium carbonate, pulverizing, reacting with water and carbon dioxide under 0.508-0.609 MPa to dissolve magnesium oxide into magnesium bicarbonate, filtering, and heating to obtain the final product.
3. The same amount of crystalline magnesium sulfate and crystalline sodium carbonate were dissolved in 10 times the amount of water, and the mixture was heated to 60 to 80 ℃ to be sufficiently mixed, thereby generating CO2 gas and simultaneously generating a precipitate. Filtering out the precipitate, mixing with hot water at 70-80 ℃, and filtering again. The washing process is repeated, and the precipitate is fully washed and then dried at 50-60 ℃.
The magnesite resources are deficient in China, the dolomite raw material is high in price, magnesium sulfate belongs to the intermediate product with high treatment price, the magnesium sulfate is prepared from sulfuric acid and is difficult to pass in environmental protection, a large amount of domestic serpentine is a good magnesium compound raw material, the price is low, the magnesium content is high, and the serpentine for preparing magnesium carbonate has various advantages. Therefore, a low-cost, high-efficiency and environment-friendly production process of light magnesium carbonate and light magnesium oxide is provided to solve the problems.
Disclosure of Invention
The invention aims to provide a low-cost, high-efficiency and environment-friendly light magnesium carbonate and light magnesium oxide production process aiming at the defects of the prior art, and the low-cost, high-efficiency and environment-friendly light magnesium carbonate and light magnesium oxide production process can well solve the problems.
In order to meet the requirements, the technical scheme adopted by the invention is as follows: the production process of the light magnesium carbonate and the light magnesium oxide with low cost, high efficiency and environmental protection comprises the following steps:
s1: crushing, fine grinding and wet deironing serpentine to obtain serpentine slurry, carrying out filter pressing, drying, feeding into a calcining furnace, calcining, cooling, crushing and feeding into a hydration tank;
s2: the temperature of the hydration tank is more than or equal to 80 ℃, the time is more than or equal to 1h, and the solid-liquid ratio of the hydration slurry is 4: 1, the stirring speed is more than or equal to 150r/min, and the solid-liquid ratio of the hydrated slurry is kept at 10: 1, sending the mixture into an aging pool, standing for 2 hours, and then sending the mixture into a carbonizer;
s3: feeding CO2 through the bottom of the carbonizer, feeding the mixed slurry into a filter press for solid-liquid separation to obtain a solid phase of low-magnesium silicon material, precipitating and purifying the filtrate to obtain solid particles with mass concentration<1g/m 3 The purified filtrate is sent into a pyrolysis furnace;
s4: heating and boiling the pyrolysis furnace, transferring the hot slurry to a large-capacity sedimentation tank, standing, settling, concentrating and collecting a solid phase;
s5: and (3) feeding the concentrated solid phase into a filter press for dehydration, drying the obtained filter cake to obtain a light magnesium carbonate product, feeding the filtrate into a blending water tank for recycling, and feeding part of light magnesium carbonate into a calcining furnace for calcination to obtain the light magnesium oxide product.
The production process of the light magnesium carbonate and the light magnesium oxide with low cost, high efficiency and environmental protection has the advantages that:
compared with a sulfuric acid method, a hydrochloric acid method and an ammonium salt method, the method does not generate new compounds, thoroughly ensures the purity of the raw materials, can easily obtain high-quality light magnesium carbonate with MgO more than or equal to 42 percent and high-quality light magnesium oxide with MgO more than or equal to 98 percent, has the advantages of environmental protection, low calcination temperature, short reaction time, mild reaction conditions, high recovery rate and the like, and is suitable for industrial production.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application is further described in detail with reference to specific embodiments below.
In the following description, references to "one embodiment," "an embodiment," "one example," "an example," etc., indicate that the embodiment or example so described may include a particular feature, structure, characteristic, property, element, or limitation, but every embodiment or example does not necessarily include the particular feature, structure, characteristic, property, element, or limitation. Moreover, repeated use of the phrase "in accordance with an embodiment of the present application" although it may possibly refer to the same embodiment, does not necessarily refer to the same embodiment.
Certain features that are well known to those skilled in the art have been omitted from the following description for the sake of simplicity.
According to one embodiment of the application, the production process of the light magnesium carbonate and the light magnesium oxide with low cost, high efficiency and environmental protection is provided, and comprises the following steps:
s1: crushing, fine grinding and wet deferrization of serpentine to obtain serpentine slurry, carrying out filter pressing, drying, calcining in a calcining furnace, cooling, crushing and then feeding into a hydration tank;
s2: the temperature of the hydration tank is more than or equal to 80 ℃, the time is more than or equal to 1h, and the solid-liquid ratio of the hydration slurry is 4: 1, the stirring speed is more than or equal to 150r/min, and the solid-liquid ratio of the hydrated slurry is kept at 10: 1, sending the mixture into an aging tank, standing for 2 hours, and then sending the mixture into a carbonizer;
s3: feeding CO2 through the bottom of the carbonizer, feeding the mixed slurry into a filter press for solid-liquid separation, wherein the solid phase is a low-magnesium silicon material, and precipitating and purifying the filtrate to ensure that the mass concentration of solid particles is high<1g/m 3 Feeding the purified filtrate into a pyrolysis furnace;
s4: heating and boiling the pyrolysis furnace, transferring the hot slurry to a large-capacity sedimentation tank, standing, settling, concentrating and collecting a solid phase;
s5: and (3) feeding the concentrated solid phase into a filter press for dehydration, drying the obtained filter cake to obtain a light magnesium carbonate product, feeding the filtrate into a blending water tank for recycling, and feeding part of light magnesium carbonate into a calcining furnace for calcination to obtain the light magnesium oxide product.
According to one embodiment of the application, the production process of the light magnesium carbonate and the light magnesium oxide with low cost, high efficiency and environmental protection specifically comprises the following steps:
1. crushing, fine grinding and wet deferrization of serpentine to obtain serpentine slurry with Tfe less than or equal to 0.5%, carrying out filter pressing, drying, sending into a calcining furnace, carrying out continuous calcination for 0.5-1h at the temperature of 550-;
2. the temperature of the hydration tank is more than or equal to 80 ℃, the time is more than or equal to 1h, and the solid-liquid ratio of the hydration slurry is 4: 1, the stirring speed is more than or equal to 150r/min, and the solid-liquid ratio of the hydrated slurry is kept at 10: 1, sending the mixture into an aging pool, standing for 2 hours, and then sending the mixture into a carbonizer;
3. feeding CO2 through the bottom of a carbonizer, keeping the pressure not less than 0.25Mpa and the temperature not more than 30 ℃, keeping the reaction time at 20Min, feeding the mixed slurry into a filter press for solid-liquid separation, wherein the solid phase is a low-magnesium silicon material, and precipitating and purifying the filtrate to ensure that the mass concentration of solid particles is high<1g/m 3 Feeding the purified filtrate into a pyrolysis furnace;
4. heating and boiling in a pyrolysis furnace for more than or equal to 10min, transferring the hot slurry to a large-capacity sedimentation tank, standing, precipitating, concentrating, and collecting a solid phase;
5. and (3) feeding the concentrated solid phase into a filter press for dehydration, drying the obtained filter cake at the temperature of less than or equal to 250 ℃ for more than or equal to 3 hours to obtain a light magnesium carbonate product, and feeding the filtrate into a blending water tank for recycling, wherein part of the light magnesium carbonate is selected and fed into a calcining furnace at the temperature of less than or equal to 800 ℃ for more than or equal to 2 hours to obtain the light magnesium oxide product.
According to one embodiment of the application, the production process of the light magnesium carbonate and the light magnesium oxide with low cost, high efficiency and environmental protection specifically comprises the following steps: crushing, fine grinding and wet deferrization of serpentine to obtain serpentine slurry with Tfe of less than or equal to 0.5%, filter pressing, drying, sending into a calcining furnace, subjecting to 550-700 ℃, continuously calcining for 0.5-1h, cooling, crushing, sending into a hydration tank, wherein the temperature of the hydration tank is more than or equal to 65 ℃, the time is more than or equal to 1h, and the solid-to-liquid ratio of the hydration slurry is 4: 1, the stirring speed is more than or equal to 150r/min, and the solid-liquid ratio of the hydrated slurry is kept at 10: 1, sending the mixture into an aging tank, standing for 2 hours, sending the mixture into a carbonizer, sending CO2 through the bottom of the carbonizer, keeping the pressure at more than or equal to 0.25Mpa and the temperature at less than or equal to 30 ℃, keeping the reaction time at 20Min, sending the mixed slurry into a filter press for solid-liquid separation, wherein the solid phase is a low-magnesium silicon material, precipitating and purifying the filtrate to ensure that the mass concentration of solid particles is less than one gram per cubic meter, sending the purified filtrate into a pyrolysis furnace, heating and boiling the pyrolysis furnace, keeping the boiling duration at more than or equal to 10Min, transferring the hot slurry into a large-capacity sedimentation tank, standing, precipitating, concentrating, collecting the solid phase, sending the concentrated solid phase into the filter press for dehydration, drying the obtained filter cake at less than or equal to 250 ℃ for more than or equal to 3 hours to obtain a light magnesium carbonate product, sending the filtrate into a blending water tank for recycling, wherein a part of light magnesium carbonate is selected and sent into a calciner at less than or equal to 800 ℃ for more than or equal to 2 hours to obtain a light magnesium oxide product, wherein the content of the magnesium oxide is more than or equal to 92 percent, and the recovery rate is more than or equal to 40 percent.
According to one embodiment of the application, the production process of the light magnesium carbonate and the light magnesium oxide with low cost, high efficiency and environmental protection specifically comprises the following steps: crushing, fine grinding and wet deferrization of serpentine to obtain serpentine slurry with Tfe of less than or equal to 0.5%, filter pressing, drying, sending into a calcining furnace, passing through 550 ℃ for 700 ℃, continuously calcining by 0.5-1, cooling, crushing, sending into a hydration tank, wherein the temperature of the hydration tank is more than or equal to 80 ℃, the time is more than or equal to 1h, and the solid-to-liquid ratio of the hydration slurry is 4: 1, the stirring speed is more than or equal to 150r/min, and the solid-liquid ratio of the hydrated slurry is kept at 10: 1, sending the mixture into an aging tank, standing for 2 hours, sending the mixture into a carbonizer, sending CO2 through the bottom of the carbonizer, keeping the pressure at more than or equal to 0.25Mpa and the temperature at less than or equal to 30 ℃, keeping the reaction time at 20Min, sending the mixed slurry into a filter press for solid-liquid separation, wherein the solid phase is a low-magnesium silicon material, precipitating and purifying the filtrate to ensure that the mass concentration of solid particles is less than one gram per cubic meter, sending the purified filtrate into a pyrolysis furnace, heating and boiling the pyrolysis furnace, keeping the boiling duration at more than or equal to 10Min, transferring the hot slurry into a large-capacity sedimentation tank, standing, precipitating, concentrating, collecting the solid phase, sending the concentrated solid phase into the filter press for dehydration, drying the obtained filter cake at less than or equal to 250 ℃ for more than or equal to 3 hours to obtain a light magnesium carbonate product, sending the filtrate into a blending water tank for recycling, wherein a part of light magnesium carbonate is selected and sent into a calciner at less than or equal to 800 ℃ for more than or equal to 2 hours to obtain a light magnesium oxide product, wherein the content of the magnesium oxide is more than or equal to 97.5 percent, and the recovery rate is more than or equal to 75 percent.
According to one embodiment of the application, the production process of the light magnesium carbonate and the light magnesium oxide with low cost, high efficiency and environmental protection specifically comprises the following steps: crushing, fine grinding and wet deferrization of serpentine to obtain serpentine slurry with Tfe of less than or equal to 0.5%, filter pressing, drying, sending into a calcining furnace, subjecting to 550-700 ℃, continuously calcining for 0.5-1h, cooling, crushing, sending into a hydration tank, wherein the temperature of the hydration tank is more than or equal to 95 ℃, the time is more than or equal to 1h, and the solid-to-liquid ratio of the hydration slurry is 4: 1, the stirring speed is more than or equal to 150r/min, and the solid-liquid ratio of the hydrated slurry is kept at 10: 1, sending the mixture into an aging tank, standing for 2 hours, sending the mixture into a carbonizer, sending CO2 through the bottom of the carbonizer, keeping the pressure at more than or equal to 0.25Mpa and the temperature at less than or equal to 30 ℃, keeping the reaction time at 20Min, sending the mixed slurry into a filter press for solid-liquid separation, wherein the solid phase is a low-magnesium silicon material, precipitating and purifying the filtrate to ensure that the mass concentration of solid particles is less than one gram per cubic meter, sending the purified filtrate into a pyrolysis 3 rd page furnace, the pyrolysis furnace is heated and boiled, the boiling duration is more than or equal to 10Min, transferring the hot slurry into a large-capacity sedimentation tank, standing, precipitating, concentrating, collecting the solid phase, sending the concentrated solid phase into the filter press for dehydration, drying the obtained filter cake at less than or equal to 250 ℃ for more than or equal to 3 hours to obtain a light magnesium carbonate product, sending the filtrate into a blending water tank for recycling, wherein a part of the light magnesium carbonate is selected and sent into a calciner, the temperature at less than or equal to 800 ℃, the time at more than or equal to 2 hours to obtain a light magnesium oxide product, wherein the content of the magnesium oxide is more than or equal to 97.2 percent, and the recovery rate is more than or equal to 76 percent.
The above-mentioned embodiments only show some embodiments of the present invention, and the description thereof is more specific and detailed, but should not be construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the claims.
Claims (6)
1. The production process of the light magnesium carbonate and the light magnesium oxide with low cost, high efficiency and environmental protection is characterized by comprising the following steps:
s1: crushing, fine grinding and wet deironing serpentine to obtain serpentine slurry, carrying out filter pressing, drying, feeding into a calcining furnace, calcining, cooling, crushing and feeding into a hydration tank;
s2: the temperature of the hydration tank is more than or equal to 80 ℃, the time is more than or equal to 1h, and the solid-liquid ratio of the hydration slurry is 4: 1, the stirring speed is more than or equal to 150r/min, and the solid-liquid ratio of the hydrated slurry is kept at 10: 1, sending the mixture into an aging pool, standing for 2 hours, and then sending the mixture into a carbonizer;
s3: feeding CO2 through the bottom of the carbonizer, feeding the mixed slurry into a filter press for solid-liquid separation, wherein the solid phase is a low-magnesium silicon material, and precipitating and purifying the filtrate to ensure that the mass concentration of solid particles is high<1g/m 3 After purificationThe filtrate is sent into a pyrolysis furnace;
s4: heating and boiling the pyrolysis furnace, transferring the hot slurry to a large-capacity sedimentation tank, standing, settling, concentrating and collecting a solid phase;
s5: and (3) feeding the concentrated solid phase into a filter press for dehydration, drying the obtained filter cake to obtain a light magnesium carbonate product, feeding the filtrate into a blending water tank for recycling, and feeding part of light magnesium carbonate into a calcining furnace for calcination to obtain the light magnesium oxide product.
2. The production process of light magnesium carbonate and light magnesium oxide with low cost, high efficiency and environmental protection as claimed in claim 1, is characterized in that: tfe in the serpentine slurry in the step S1 is less than or equal to 0.5 percent.
3. The production process of light magnesium carbonate and light magnesium oxide with low cost, high efficiency and environmental protection as claimed in claim 1, is characterized in that: the temperature of the calcining furnace in the step S1 is 550-700 ℃, and the forging time is 0.5-1 h.
4. The production process of light magnesium carbonate and light magnesium oxide with low cost, high efficiency and environmental protection as claimed in claim 1, is characterized in that: in step S3, the pressure of the carbonizer is maintained to be more than or equal to 0.25Mpa, the temperature is kept to be less than or equal to 30 ℃, and the reaction time is kept to be 20 Min.
5. The production process of light magnesium carbonate and light magnesium oxide with low cost, high efficiency and environmental protection as claimed in claim 1, is characterized in that: the boiling duration is more than or equal to 10min in step S4.
6. The production process of light magnesium carbonate and light magnesium oxide with low cost, high efficiency and environmental protection as claimed in claim 1, is characterized in that: in the step S5, the drying temperature of the filter cake is less than or equal to 250 ℃, the time is more than or equal to 3 hours, the temperature of the calcining furnace is less than or equal to 800 ℃, and the calcining time is more than or equal to 2 hours.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB595284A (en) * | 1944-11-02 | 1947-12-01 | Marine Magnesium Products Corp | Process for production of magnesium carbonate |
| CN1865140A (en) * | 2005-05-19 | 2006-11-22 | 王斌俊 | Nemalite carbonization for preparing light magnesium carbonate and high purity magnesia |
| KR20130036893A (en) * | 2011-10-05 | 2013-04-15 | 한국지질자원연구원 | A method for sequestration of carbon dioxide by synthesis of magnesite from serpentine |
| CN103910366A (en) * | 2014-04-17 | 2014-07-09 | 宁婷婷 | Method for preparing high-purity magnesium oxide by utilizing serpentinite |
| CN107915242A (en) * | 2017-05-30 | 2018-04-17 | 张旭 | Asbestos tailings prepare method of magnesium oxide |
-
2022
- 2022-07-18 CN CN202210841019.3A patent/CN115124055A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB595284A (en) * | 1944-11-02 | 1947-12-01 | Marine Magnesium Products Corp | Process for production of magnesium carbonate |
| CN1865140A (en) * | 2005-05-19 | 2006-11-22 | 王斌俊 | Nemalite carbonization for preparing light magnesium carbonate and high purity magnesia |
| KR20130036893A (en) * | 2011-10-05 | 2013-04-15 | 한국지질자원연구원 | A method for sequestration of carbon dioxide by synthesis of magnesite from serpentine |
| CN103910366A (en) * | 2014-04-17 | 2014-07-09 | 宁婷婷 | Method for preparing high-purity magnesium oxide by utilizing serpentinite |
| CN107915242A (en) * | 2017-05-30 | 2018-04-17 | 张旭 | Asbestos tailings prepare method of magnesium oxide |
Non-Patent Citations (1)
| Title |
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| 代厚全等: "从蛇纹石制备轻质碳酸镁和轻质氧化镁的扩试研究", 《四川师范大学学报（自然科学版）》, vol. 21, no. 2, pages 192 - 195 * |
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