CN110844924B - Method for producing food-grade and feed-grade anhydrous magnesium sulfate - Google Patents
Method for producing food-grade and feed-grade anhydrous magnesium sulfate Download PDFInfo
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- CN110844924B CN110844924B CN201911225093.7A CN201911225093A CN110844924B CN 110844924 B CN110844924 B CN 110844924B CN 201911225093 A CN201911225093 A CN 201911225093A CN 110844924 B CN110844924 B CN 110844924B
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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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Abstract
The invention discloses a method for producing food-grade and feed-grade anhydrous magnesium sulfate, which comprises the steps of reaction, filtration, spray drying, polymerization drying, cooling and packaging and the like; the invention has the advantages that: the production process is short, the spray drying time is only 10-30 seconds, the product can keep uniform and fine particles due to the short drying time, the product has good dispersibility, fluidity and solubility, a large amount of energy is saved, and the production cost is reduced. The drying effect is good, and the liquid can be dried into a powdery product at one time without crushing and screening.
Description
Technical Field
The invention relates to a preparation method of magnesium sulfate, in particular to a method for producing food-grade and feed-grade anhydrous magnesium sulfate, belonging to the field of food additives and feeds.
Background
Magnesium is used in food additives for nutritional supplements, firming agents, flavor enhancers, and is also an essential nutrient for humans and animals, and magnesium deficiency in humans and animals causes numerous diseases. The anhydrous magnesium sulfate is not agglomerated, is convenient to store and is more and more widely applied, and the research on the production method of the anhydrous magnesium sulfate with short process and low cost has important significance.
The existing food-grade and feed-grade magnesium sulfate is mainly food-grade magnesium sulfate heptahydrate and is generally prepared by dissolving and recrystallizing industrial-grade magnesium sulfate. The process is carried out by cooling and crystallizing to generate magnesium sulfate heptahydrate, dissolving magnesium sulfate heptahydrate, recrystallizing and drying, and has the advantages of complex process, high energy consumption and high production cost.
Disclosure of Invention
The invention aims to design a method for producing food-grade and feed-grade anhydrous magnesium sulfate, which has short production flow, saves a large amount of energy and reduces the production cost.
The technical scheme of the invention is as follows:
a method for producing food grade, feed grade anhydrous magnesium sulfate, comprising the steps of:
(1) reaction: adding magnesia powder and concentrated sulfuric acid into a reactor for reaction to generate saturated magnesium sulfate solution with the specific gravity of 1.40-1.44g/cm3；
(2) And (3) filtering: filtering the reaction product obtained in the step (1) by a filter press to remove impurities to obtain a saturated solution;
(3) spray drying: the saturated solution obtained in the step (2) enters an intermediate tank, then the solution is sent to a high-speed centrifugal atomizer at the top of the drying tower by a screw pump, and an atomizing disc of the atomizer atomizes the feed liquid into fog drops in a high-speed rotating and uniform manner;
High-temperature hot air supplied by a natural gas device enters a drying chamber of a spray drying tower from the top, the heated temperature is 300-450 ℃, the hot air enters spray drying equipment at a proper and uniform wind speed of 18-22m/s to contact with magnesium sulfate solution for initial mass and heat exchange, feed liquid is rotated and sprayed into ultrafine atomized liquid beads through a high-speed centrifugal atomizer at the top of a tower body to contact with the hot air, moisture rapidly absorbs heat transferred by the hot air and is gasified, so that solute magnesium sulfate is separated from the moisture, finished magnesium sulfate is continuously output and collected from the bottom of the drying tower and a cyclone separator, water vapor is rapidly discharged, and MgSO (MgSO) is obtained by drying4·2H2O；
(4) Polymerization and drying: MgSO (MgSO) in vitro4·2H2O, conveying the materials into a polymerization drying tower through a screw conveyor to perform sufficient heat exchange with high-temperature hot air provided by a natural gas hot blast stove, and completing the drying process of anhydrous magnesium sulfate;
(5) cooling and packaging: and (4) cooling the dried finished product to below 40 ℃ in a cooler, and directly packaging the cooled product in a packaging system to obtain the final product anhydrous magnesium sulfate.
The weight ratio of the magnesia powder to the concentrated sulfuric acid in the step (1) is 1: 2.3-3.
The mass concentration of the sulfuric acid is 93-98%.
The invention adopts two identical neutralization reactors with stirring devices, namely a reactor for reacting magnesium oxide with concentrated sulfuric acid to generate saturated magnesium sulfate solution, and adopts a drying technology combining spray drying and polymerization drying to ensure that continuous production of the spray drying and the polymerization drying is not interrupted.
The beneficial effects of the invention are as follows: the production process is short, the spray drying time is only 10-30 seconds, the product can keep uniform and fine particles due to the short drying time, the product has good dispersibility, fluidity and solubility, a large amount of energy is saved, and the production cost is reduced. The drying effect is good, and the liquid can be dried into a powdery product at one time without crushing and screening.
The invention is further illustrated by the following examples in conjunction with the drawings.
Drawings
FIG. 1 is a process flow diagram of an embodiment of the present invention.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1
26000kg of water is added into a reactor, 11000kg of magnesia powder is added under the stirring state, 2990kg of 93 percent sulfuric acid is added for reaction, the reaction time is controlled to be 4 hours, the temperature is controlled to be 80-90 ℃, and when the pH is 5-7, the reaction reaches the end point. Then filtering by a filter press, feeding the filtrate into an intermediate storage tank, pumping the filtrate into a spray drying tower by using a screw metering pump to obtain magnesium sulfate dihydrate 1.31 t/h, and feeding the generated magnesium sulfate dihydrate into a polymerization drying tower to obtain the anhydrous magnesium sulfate product with the yield of 1 t/h.
Example 2
26150kg of water is added into a reactor, 11000kg of magnesium oxide powder is added under the stirring state, 2837kg of 98 percent sulfuric acid is added for reaction, the reaction time is controlled to be 5 hours, the temperature is controlled to be 80-90 ℃, and when the pH is 5-7, the reaction reaches the end point. Then filtering by a filter press, pumping into a spray drying tower by a screw metering pump to obtain magnesium sulfate dihydrate 1.31 t/h, and feeding the generated magnesium sulfate dihydrate into a polymerization drying tower to obtain anhydrous magnesium sulfate with the yield of 1 t/h.
Claims (1)
1. A method for producing food-grade and feed-grade anhydrous magnesium sulfate is characterized by comprising the following steps:
(1) reaction: adding magnesia powder and concentrated sulfuric acid into a reactor for reaction to generate saturated magnesium sulfate solution with the specific gravity of 1.40-1.44g/cm3；
(2) And (3) filtering: filtering the reaction product obtained in the step (1) by a filter press to remove impurities to obtain a saturated solution;
(3) spray drying: the saturated solution obtained in the step (2) enters an intermediate tank, then the solution is sent to a high-speed centrifugal atomizer at the top of the drying tower by a screw pump, and an atomizing disc of the atomizer atomizes the feed liquid into fog drops in a high-speed rotating and uniform manner;
high-temperature hot air supplied by a natural gas device enters a drying chamber of a spray drying tower from the top, the heating temperature is 300- 4·2H2O；
(4) Polymerization and drying: MgSO (MgSO)4·2H2Conveying the materials into a polymerization drying tower through a screw conveyor to perform sufficient heat exchange with high-temperature hot air provided by a natural gas hot-blast stove, and completing the drying process of anhydrous magnesium sulfate;
(5) cooling and packaging: cooling the dried finished product to below 40 ℃ in a cooler, and directly packaging the cooled product in a packaging system to obtain a final product anhydrous magnesium sulfate;
the weight ratio of the magnesia powder to the concentrated sulfuric acid in the step (1) is 1: 2.3-3;
the mass concentration of the sulfuric acid is 93-98%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911225093.7A CN110844924B (en) | 2019-12-04 | 2019-12-04 | Method for producing food-grade and feed-grade anhydrous magnesium sulfate |
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| CN201911225093.7A CN110844924B (en) | 2019-12-04 | 2019-12-04 | Method for producing food-grade and feed-grade anhydrous magnesium sulfate |
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| CN110844924A CN110844924A (en) | 2020-02-28 |
| CN110844924B true CN110844924B (en) | 2022-06-10 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0652180B1 (en) * | 1991-06-10 | 1997-05-21 | Exportadora De Sal S.A. De C.V. | Method for recovering magnesium sulfate products from mixtures of epsomite and halite |
| CN103708509A (en) * | 2013-12-20 | 2014-04-09 | 杨海基 | Method for producing magnesium sulfate monohydrate by using spray drying process |
| CN105399116B (en) * | 2015-11-16 | 2017-07-25 | 中国科学院过程工程研究所 | A kind of processing system of spent acid containing organic matter and its processing method and purposes |
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2019
- 2019-12-04 CN CN201911225093.7A patent/CN110844924B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0652180B1 (en) * | 1991-06-10 | 1997-05-21 | Exportadora De Sal S.A. De C.V. | Method for recovering magnesium sulfate products from mixtures of epsomite and halite |
| CN103708509A (en) * | 2013-12-20 | 2014-04-09 | 杨海基 | Method for producing magnesium sulfate monohydrate by using spray drying process |
| CN105399116B (en) * | 2015-11-16 | 2017-07-25 | 中国科学院过程工程研究所 | A kind of processing system of spent acid containing organic matter and its processing method and purposes |
Non-Patent Citations (1)
| Title |
|---|
| 湿式镁法烟气脱硫副产物MgSO4热解回收MgO;亢万忠等;《化工环保》;20121231;第32卷(第1期);第57-60页 * |
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