CN115353131B - Production method of magnesium sulfate monohydrate - Google Patents
Production method of magnesium sulfate monohydrate Download PDFInfo
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- CN115353131B CN115353131B CN202211141629.9A CN202211141629A CN115353131B CN 115353131 B CN115353131 B CN 115353131B CN 202211141629 A CN202211141629 A CN 202211141629A CN 115353131 B CN115353131 B CN 115353131B
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- magnesium sulfate
- sulfuric acid
- concentrated sulfuric
- sulfate heptahydrate
- magnesium
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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
- C01F5/40—Magnesium sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/1045—Oxyacids
- C01B35/1054—Orthoboric acid
- C01B35/1063—Preparation from boron ores or borates using acids or salts
Abstract
The invention provides a method for producing magnesium sulfate monohydrate, which belongs to the technical field of magnesium sulfate production and comprises the following steps: mixing the magnesium sulfate heptahydrate with concentrated sulfuric acid, and crystallizing to obtain magnesium sulfate monohydrate. The invention takes magnesium sulfate heptahydrate as raw material, takes concentrated sulfuric acid as dehydrating agent, and after the magnesium sulfate heptahydrate is mixed with the concentrated sulfuric acid, the magnesium sulfate heptahydrate is continuously dissolved in the self crystallization water, at the moment, the concentration of the concentrated sulfuric acid is rapidly reduced, the magnesium sulfate reaches the saturation rate to crystallize magnesium sulfate monohydrate and takes the magnesium sulfate heptahydrate as seed crystal to complete the crystallization process. The results of the examples show that the magnesium sulfate monohydrate produced by the production method of the invention accords with the specification of magnesium sulfate for agriculture GB/T26568-2011.
Description
Technical Field
The invention relates to the technical field of magnesium sulfate production, in particular to a production method of magnesium sulfate monohydrate.
Background
Magnesium sulfate can be classified into: anhydrous magnesium sulfate (MgSO) 4 ) Magnesium sulfate monohydrate (MgSO) 4 ·H 2 O), magnesium sulfate heptahydrate (MgSO) 4 ·7H 2 O), magnesium sulfate hexahydrate (MgSO) 4 ·6H 2 O), and the like, wherein the commercial magnesium sulfate is mainly the first three. The magnesium sulfate heptahydrate is relatively simple to synthesize, low in cost and high in market share; the chemical synthesis of magnesium sulfate monohydrate and anhydrous magnesium sulfate is complex and the cost is high; magnesium sulfate hexahydrate is not seen in the market because it has little advantage in product performance.
Magnesium sulfate monohydrate is an important inorganic agricultural product and is mainly applied to feed, fertilizer industry, food moisture absorbent and the like in China at present. The magnesium sulfate low-hydrate is used as a ruminant feed additive, and can effectively promote animal digestion and protease synthesis; when the compound fertilizer is manufactured, magnesium sulfate monohydrate is used as a drying additive (anti-caking agent), so that the magnesium content is high, the transportation cost is low, the product performance can be obviously improved, the phenomenon of hardening and blocking can not occur in the storage and transportation process, and the compound fertilizer is an indispensable raw material for manufacturing trace element water-soluble fertilizers.
The magnesium sulfate monohydrate mainly comprises the following synthetic methods: one is to crystallize water-soluble magnesium salt in an autoclave to prepare a purer product, but the crystallization temperature reaches 180 ℃, the crystallization is needed to be carried out in the autoclave, the operation condition is harsh, the energy consumption is high, and the preferential process consideration is not generally needed; the other light burned powder formed by magnesite Dan Duanshao is directly mixed and reacted with concentrated sulfuric acid to prepare the magnesium sulfate, the method has simple process flow and low cost, but because the product contains insoluble magnesium oxide which is not fully reacted, the water insoluble matters generally account for about 15 percent of the product, and the product is only suitable for being used as a non-fully water soluble medium element fertilizer and cannot meet the requirement of magnesium sulfate for agriculture; therefore, most of the domestic production of the full water-soluble magnesium sulfate monohydrate at present adopts a high-temperature forced dehydration process of the magnesium sulfate heptahydrate, but the method has the defects of higher temperature (400 ℃ required), high pressure condition and high energy consumption, thereby limiting the development of the method.
Therefore, how to reduce the production temperature and pressure when preparing magnesium sulfate monohydrate from magnesium sulfate heptahydrate, thereby reducing the energy consumption becomes a difficult problem in the existing production of magnesium sulfate monohydrate.
Disclosure of Invention
The invention aims to provide a method for producing magnesium sulfate monohydrate. The production method provided by the invention can be carried out at normal pressure and lower temperature, and has lower energy consumption.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for producing magnesium sulfate monohydrate, which comprises the following steps:
mixing the magnesium sulfate heptahydrate with concentrated sulfuric acid, and crystallizing to obtain magnesium sulfate monohydrate.
Preferably, the mass concentration of the concentrated sulfuric acid is 85-93%.
Preferably, the temperature of the concentrated sulfuric acid is 40-90 ℃.
Preferably, the ratio of the amount of the magnesium sulfate heptahydrate to the amount of the sulfuric acid in the concentrated sulfuric acid is 1: (0.8-1.4).
Preferably, the ratio of the amount of the magnesium sulfate heptahydrate to the amount of the sulfuric acid in the concentrated sulfuric acid is 1: (0.9-1.2).
Preferably, the temperature of the crystallization is 50 to 80 ℃.
Preferably, the temperature of the crystallization is 50 to 60 ℃.
Preferably, the crystallization time is 30 to 45 minutes.
Preferably, primary filtrate is obtained after crystallization, and the primary filtrate is mixed with boron-magnesium mineral powder and then subjected to pre-acidolysis to obtain a pre-acidolysis material; the pre-acidolysis material is used for preparing boric acid by a boron magnesium mineral powder one-step method.
Preferably, the volume ratio of the mass of the boron magnesium mineral powder to the primary filtrate is (4.5-5.0) t/m 3 。
The invention provides a method for producing magnesium sulfate monohydrate, which comprises the following steps: mixing the magnesium sulfate heptahydrate with concentrated sulfuric acid, and crystallizing to obtain magnesium sulfate monohydrate. The invention takes magnesium sulfate heptahydrate as raw material, takes concentrated sulfuric acid as dehydrating agent, and after the magnesium sulfate heptahydrate is mixed with the concentrated sulfuric acid, the magnesium sulfate heptahydrate is continuously dissolved in the self crystallization water, at the moment, the concentration of the concentrated sulfuric acid is rapidly reduced, the magnesium sulfate reaches the saturation rate to crystallize magnesium sulfate monohydrate and takes the magnesium sulfate heptahydrate as seed crystal to complete the crystallization process. The results of the examples show that the magnesium sulfate monohydrate produced by the production method of the invention accords with the specification of magnesium sulfate for agriculture GB/T26568-2011.
Drawings
FIG. 1 is a process flow diagram of a one-step process for preparing boric acid from boron-magnesium mineral powder;
FIG. 2 is a process flow diagram of the method for producing magnesium sulfate monohydrate of the present invention.
Detailed Description
The invention provides a method for producing magnesium sulfate monohydrate, which comprises the following steps:
mixing the magnesium sulfate heptahydrate with concentrated sulfuric acid, and crystallizing to obtain magnesium sulfate monohydrate.
The source of each raw material is not particularly limited unless specifically stated, and the raw materials may be commercially available products or products prepared by conventional preparation methods, which are well known to those skilled in the art.
In the invention, the magnesium sulfate heptahydrate is preferably magnesium sulfate heptahydrate generated in the process of preparing boric acid by a boron magnesium mineral powder one-step method. In the invention, the magnesium sulfate heptahydrate is a byproduct in the process of producing boric acid by utilizing the boron magnesium ore, and the price is low.
In the invention, the process flow chart of the one-step method for preparing boric acid from the boron magnesium mineral powder is preferably as shown in fig. 1: and (3) acidolysis is carried out on concentrated sulfuric acid and boron magnesium mineral powder in an acidolysis tank, filtering is carried out sequentially through a plate-frame filter, a large-scale water tank and a crystallization tank, floatation is carried out through a floatation machine, crude boric acid and crude magnesium sulfate are obtained, boric acid is obtained after centrifugal filtration and drying of the crude boric acid, and magnesium sulfate is obtained after centrifugal filtration and drying of the crude magnesium sulfate.
In the invention, the magnesium sulfate heptahydrate generated in the process of preparing boric acid by the boron magnesium mineral powder through a one-step method is a mixture containing boron and iron; the boron content in the magnesium sulfate heptahydrate is 1-3% based on boric acid; the iron content in the magnesium sulfate heptahydrate is about 1 percent calculated by ferrous sulfate.
In the present invention, the mass concentration of the concentrated sulfuric acid is preferably 85 to 93%, more preferably 88 to 93%, and most preferably 90 to 93%. The invention limits the mass concentration of the concentrated sulfuric acid in the range, avoids the phenomenon of crystallization and peptone in winter in the north, causes the fluid in the pipeline not to flow, influences the production, simultaneously avoids the concentration of the concentrated sulfuric acid to be too low, influences the crystallization efficiency of magnesium sulfate monohydrate, and increases the water quantity to be evaporated for the adsorption process due to the low concentration of primary filtrate.
In the present invention, the temperature of the concentrated sulfuric acid is preferably 40 to 90 ℃, more preferably 50 to 90 ℃, and most preferably 70 to 90 ℃. The invention limits the temperature of the concentrated sulfuric acid to the above range, and the higher temperature can accelerate the dissolution speed of the magnesium sulfate heptahydrate and improve the production efficiency.
In the present invention, the ratio of the amount of the magnesium sulfate heptahydrate to the amount of the sulfuric acid in the concentrated sulfuric acid is preferably 1: (0.8 to 1.4), more preferably 1: (0.9 to 1.3), most preferably 1: (1.0-1.2). The invention limits the ratio of the amounts of substances of the magnesium sulfate heptahydrate and the sulfuric acid in the concentrated sulfuric acid to the above range, the sulfuric acid after mixing the two has proper concentration (more than 40 percent), so that the magnesium sulfate is saturated, and the magnesium sulfate monohydrate is obtained after crystallization due to the homoionic effect; meanwhile, when the obtained primary filtrate is mixed with the boron magnesium mineral powder, a large amount of heat can be released, redundant water is evaporated, and the obtained pre-acidolysis material is reused in the boric acid preparation process without adding redundant water to the boric acid circulating mother liquor and damaging the mother liquor balance.
In the present invention, the mixing of the magnesium sulfate heptahydrate with the concentrated sulfuric acid is preferably: firstly, heating concentrated sulfuric acid to 40-90 ℃, and then adding magnesium sulfate heptahydrate.
In the present invention, the temperature of the crystallization is preferably 50 to 80 ℃, more preferably 50 to 70 ℃, and most preferably 50 to 60 ℃; the time for the crystallization is preferably 30 to 45 minutes, more preferably 30 to 40 minutes. The invention limits the crystallization temperature and time to the above range, so that the magnesium sulfate heptahydrate can be fully crystallized to form magnesium sulfate monohydrate. In the crystallization process, magnesium sulfate heptahydrate is continuously dissolved in self crystallization water at a higher temperature, the concentration of sulfuric acid is rapidly reduced, when the concentration of sulfuric acid is not changed any more, magnesium sulfate reaches saturation, magnesium sulfate monohydrate is crystallized first and is used as seed crystal, the whole crystallization process is completed, the solubility of magnesium sulfate is much smaller than that of magnesium sulfate monohydrate due to the homoionic effect, and when the concentration of sulfuric acid is more than 40%, the crystallized product is magnesium sulfate monohydrate.
In the present invention, the crystallization is preferably performed under stirring. The stirring rate is not particularly limited in the present invention, and a stirring rate conventional in the art may be used.
After the crystallization is completed, the crystallized product is preferably filtered, washed and dried in sequence to obtain the magnesium sulfate monohydrate.
The filtering operation is not particularly limited in the present invention, and filtering techniques well known to those skilled in the art may be employed.
In the present invention, the reagent used for the washing is preferably a saturated solution of magnesium sulfate at 50 to 90 ℃. The invention adopts 50-90 ℃ magnesium sulfate saturated solution for washing, the hot saturated solution can thoroughly wash impurity sulfuric acid with less consumption, and meanwhile, when the impurity sulfuric acid enters into washing liquid (secondary filtrate), the impurity sulfuric acid and light burned powder containing magnesium oxide are subjected to neutralization reaction, and the temperature is high and the reaction is fast.
The drying operation is not particularly limited, and a drying scheme well known to those skilled in the art may be adopted.
In the present invention, the crystallization is preferably followed by a primary filtrate. In the present invention, the primary filtrate is preferably obtained by filtering the crystallized product.
The method is characterized in that the primary filtrate is mixed with boron-magnesium mineral powder and then subjected to pre-acidolysis to obtain a pre-acidolysis material; the pre-acidolysis material is used for preparing boric acid by a boron magnesium mineral powder one-step method.
The invention is not particularly limited in the kind of the boromagnesium mineral powder, and the boromagnesium mineral powder for producing boric acid, which is well known to those skilled in the art, can be adopted.
In the invention, the volume ratio of the mass of the boron magnesium mineral powder to the primary filtrate is preferably (4.5-5.0) t/m 3 . The invention limits the mass ratio of the boron magnesium mineral powder and the primary filtrate to the above range, can lead the two to react to release a large amount of heat, and part of carbonate escapes in the form of carbon dioxide, so that the excessive moisture is mostly evaporated, the excessive water is not added to the boric acid circulating mother liquor, the balance of the mother liquor is not destroyed, the acidolysis time can be shortened, the bubbling and can-out phenomenon caused by the escape of carbon dioxide in the acidolysis process can be eliminated, and the acidolysis rate is improved.
In the invention, the chemical reaction of the boron magnesium mineral powder and the primary filtrate is as follows:
2MgO·B 2 O 3 ·H 2 O+2H 2 SO 4 ＝2H 3 BO 3 +2MgSO 4 +H 2 O
CaCO 3 +H 2 SO 4 ＝CaSO 4 +CO 2 +H 2 O
FeO·Fe 2 O 3 +4H 2 SO 4 ＝FeSO 4 +Fe 2 (SO 4 ) 3 +4H 2 O
Mg(Si 4 O 10 )(OH) 8 +6H 2 SO 4 ＝6MgSO 4 4SiO 2 +10H 2 O。
in the invention, the pre-acidolysis material is used for preparing boric acid by a one-step method of boron magnesium mineral powder, and the preparation method is preferably as follows: and mixing the pre-acidolysis material with concentrated sulfuric acid for acidolysis and subsequent processes.
In the present invention, the secondary filtrate is preferably obtained after the washing, and after the secondary filtrate is obtained, the secondary filtrate is preferably mixed with the light burned powder and filtered to obtain a saturated solution of magnesium sulfate as a washing reagent.
In the invention, the addition amount of the light burned powder is preferably calculated according to the following formula:
wherein: x- -the amount of light burned powder added into the secondary filtrate is kg,
m- - - -weight kg of sulfuric acid in the secondary filtrate (calculated from the volume and the measured g/L concentration of sulfuric acid),
n is the percentage of the light burned powder magnesium oxide,
0.411- - -coefficient: mgO and H 2 SO 4 The ratio of the molar masses of the components,
1.05- - -coefficient: the actual adding amount of the light burned powder is 1.05 times of the theoretical adding amount.
In the invention, the light burned powder is used for neutralizing sulfuric acid in the secondary filtrate to obtain magnesium sulfate, and can be reused in a washing process to form self circulation.
In the present invention, the flow chart of the production method of magnesium sulfate monohydrate is preferably as shown in fig. 2: mixing magnesium sulfate heptahydrate with concentrated sulfuric acid in an enamel kettle, filtering by a vacuum belt filter to obtain primary filtrate and a magnesium sulfate monohydrate crude product, washing the magnesium sulfate monohydrate crude product by a saturated solution of magnesium sulfate, drying by a flash evaporation dryer to obtain a magnesium sulfate monohydrate finished product, packaging, mixing the washed secondary filtrate with light burned powder in an acid neutralization kettle, filtering by a filter, recycling the obtained saturated solution of magnesium sulfate to a washing process, and discharging filter residues.
According to the invention, magnesium sulfate heptahydrate is taken as a raw material, concentrated sulfuric acid is taken as a dehydrating agent, after the magnesium sulfate heptahydrate is mixed with the concentrated sulfuric acid, the magnesium sulfate heptahydrate is continuously dissolved in self crystallization water, the concentration of the concentrated sulfuric acid is rapidly reduced, magnesium sulfate reaches saturation rate to crystallize magnesium sulfate monohydrate, the magnesium sulfate heptahydrate is taken as seed crystal, the crystallization process is completed, the parameters such as the dosage of each component, the reaction temperature and the time are controlled, and the magnesium sulfate heptahydrate can be produced without high temperature and high pressure conditions, so that the energy consumption is low; meanwhile, the obtained primary filtrate is mixed with the boron magnesium mineral powder for pre-acidolysis, and the obtained pre-acidolysis material can be recycled to a batching system for boric acid production, so that the acidolysis rate is improved; the secondary filtrate obtained after washing the magnesium sulfate monohydrate is mixed with the light burned powder to obtain magnesium sulfate solution, which can be reused in the washing process, and the materials in the whole process can be recycled, thus reducing the production cost.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The magnesium sulfate heptahydrate of the embodiment is a byproduct magnesium sulfate heptahydrate of boric acid prepared by a one-step method of boron-magnesium mineral powder, is a mixture containing boron and iron, and is 1 percent based on boric acid and 1.2 percent based on ferrous sulfate;
specific: (1) 150mL of concentrated sulfuric acid with the mass concentration of 92.5% is added into a 1000mL beaker, and the mixture is heated to 90 ℃ on an electric furnace;
(2) Slowly adding magnesium sulfate heptahydrate (the ratio of the magnesium sulfate heptahydrate to the sulfuric acid in the concentrated sulfuric acid is 1:1.4) into a beaker, starting magnetic stirring, continuously dissolving the magnesium sulfate heptahydrate, starting to form white crystals, naturally reducing the temperature to 50 ℃, preserving heat, and stirring for 30min to finish crystallization, thus obtaining 450mL of magnesium sulfate monohydrate slurry;
(3) Transferring the slurry obtained in the step (2) to a suction bottle for vacuum suction filtration to obtain 240mL of primary filtrate and a magnesium sulfate monohydrate filter cake, and assaying and analyzing the result of the primary filtrate: sulfuric acid: the mass concentration is 49.55 percent, H 3 BO 3 :10.71g/L, magnesium sulfate: 101.4g/L;
(4) Washing magnesium sulfate monohydrate filter cake with 70deg.C and 400mL saturated magnesium sulfate solution to obtain secondary filtrate containing 182.59g/L sulfuric acid, adding light burned powder (with magnesium oxide mass content of 81.5%) and neutralizing (reaction equation: mgO+H) 2 SO 4 ＝MgSO 4 +H 2 O, the addition amount of the light burned powder is 1.05 times of the theoretical amount), the temperature is kept, the concentration of the magnesium sulfate is adjusted to be saturated, the plate frame filters impurities to obtain saturated magnesium sulfate solution, and the saturated magnesium sulfate solution can be recycled;
(5) The secondary filter cake is placed in a drying box, dried for 1.5h at 110 ℃, and weighed for 248.5g, wherein the mass content of magnesium is 16.9%, sulfuric acid is 0.02%, boric acid is 0.01%, water insoluble substances are 0.31%, and other indexes meet the specifications of agricultural magnesium sulfate GB/T26568-2011.
1170g of boron magnesium mineral powder is placed in a porcelain basin, 240mL of primary filtrate is placed in a beaker, and the mixture is slowly added into the porcelain basin in parts and stirred by a glass rod (the volume ratio of the mass of the boron magnesium mineral powder to the primary filtrate is 4.88 t/m) 3 ) The reaction of acid and mineral powder is gradually and violent, the material surface has bubbles to generate and release heat, the temperature reaches more than 90 ℃, most of water in primary filtrate is evaporated, after the reaction is finished, the water is naturally cooled to become dry small-block pre-acidolysis material, the weight is 1474.2g, the yield coefficient is 1474.2/1170=1.26, and the obtained pre-acidolysis material returns to the acidolysis batching procedure for boric acid production.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (6)
1. A method for producing magnesium sulfate monohydrate, comprising:
mixing magnesium sulfate heptahydrate with concentrated sulfuric acid, and crystallizing to obtain magnesium sulfate monohydrate;
the temperature of the concentrated sulfuric acid is 40-90 ℃; the crystallization temperature is 50-80 ℃;
a primary filtrate is also obtained after crystallization, and the primary filtrate is mixed with boron magnesium mineral powder and then subjected to pre-acidolysis to obtain a pre-acidolysis material; the pre-acidolysis material is used for preparing boric acid by a boron magnesium mineral powder one-step method; the volume ratio of the mass of the boron magnesium mineral powder to the primary filtrate is (4.5-5.0) t/m 3 ；
The pre-acidolysis material is used for preparing boric acid by a boron magnesium mineral powder one-step method, and comprises the following steps: and mixing the pre-acidolysis material with concentrated sulfuric acid for acidolysis and subsequent processes.
2. The production method according to claim 1, wherein the mass concentration of the concentrated sulfuric acid is 85 to 93%.
3. The production method according to claim 1, wherein the ratio of the amount of the magnesium sulfate heptahydrate to the amount of the sulfuric acid in the concentrated sulfuric acid is 1: (0.8-1.4).
4. A production method according to claim 3, wherein the ratio of the amount of the magnesium sulfate heptahydrate to the amount of the sulfuric acid in the concentrated sulfuric acid is 1: (0.9-1.2).
5. The method according to claim 1, wherein the crystallization temperature is 50 to 60 ℃.
6. The method according to claim 1, wherein the crystallization time is 30 to 45 minutes.
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| US4804524A (en) * | 1986-01-29 | 1989-02-14 | Materias Primas Magdalena, S.A. De C.V. | Process for the preparation of boric acid from colemanite and/or howlite minerals |
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| CN104291367A (en) * | 2014-09-28 | 2015-01-21 | 西南科技大学 | Production method of magnesium sulfate monohydrate |
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2022
- 2022-09-20 CN CN202211141629.9A patent/CN115353131B/en active Active
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| US4804524A (en) * | 1986-01-29 | 1989-02-14 | Materias Primas Magdalena, S.A. De C.V. | Process for the preparation of boric acid from colemanite and/or howlite minerals |
| CN101134589A (en) * | 2006-09-01 | 2008-03-05 | 多氟多化工股份有限公司 | Method for preparing aluminun fluoride, waterless magnesium sulfate and sodium fluoride |
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