CN112159254A - Method for joint production of magnesium oxide fiber and potassium sulfate/magnesium sulfate potash fertilizer - Google Patents
Method for joint production of magnesium oxide fiber and potassium sulfate/magnesium sulfate potash fertilizer Download PDFInfo
- Publication number
- CN112159254A CN112159254A CN202010999811.2A CN202010999811A CN112159254A CN 112159254 A CN112159254 A CN 112159254A CN 202010999811 A CN202010999811 A CN 202010999811A CN 112159254 A CN112159254 A CN 112159254A
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- Prior art keywords
- magnesium sulfate
- magnesium
- sulfate
- potassium
- magnesium oxide
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D1/00—Fertilisers containing potassium
- C05D1/02—Manufacture from potassium chloride or sulfate or double or mixed salts thereof
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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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
Abstract
The invention discloses a method for producing magnesium oxide fiber and potassium sulfate/magnesium sulfate potash fertilizer in a combined manner, and relates to a preparation method of chemical products. Adding polyethylene glycol accounting for 20.0-40.wt% of the mass of magnesium sulfate into a magnesium sulfate solution, uniformly stirring a heptahydrate magnesium sulfate solution mixed with the polyethylene glycol, and then mixing the magnesium sulfate solution and the polyethylene glycol according to the molar ratio of anhydrous potassium carbonate to magnesium sulfate of 1: 1-1.2, slowly dripping a potassium carbonate solution into the magnesium sulfate mixed solution at room temperature, stirring for 20-60min after completion, aging for two hours, filtering a reactant, wherein a filtrate is a potassium sulfate fertilizer or a magnesium sulfate potassium fertilizer, a precipitate is a precursor of magnesium oxide fibers, and calcining the washed and dried precursor to a certain temperature to prepare the magnesium oxide fibers. In the process of preparing the magnesium oxide fiber, the potassium sulfate fertilizer or the magnesium sulfate potash fertilizer is produced, no industrial waste and pollutant are generated, and the economic benefit of the product is obviously improved.
Description
Technical Field
The invention relates to a preparation method of chemical products, in particular to a method for jointly producing magnesium oxide fibers and potassium sulfate/magnesium sulfate potash fertilizers.
Background
A thermal battery is a battery that operates by heating an electrolyte to a molten state under the action of a heat source. The main use scene of thermal battery is in the military products such as guided missile, because the electrolyte is liquid under the molten condition, just lead to receiving vibrations in its use, under this condition, the electrolyte in the thermal battery is very easily exposed, this kind reveals and then can lead to the noise slightly, thereby arouse the electrolyte loss to accelerate the discharge of battery, the emergence that can lead to the battery short circuit seriously, damage components and parts, for reducing the electrolyte and flow the possibility under the molten condition, guarantee that the thermal battery normally operates under various extreme use scenes, often add the binder.
MgO has good physical and chemical properties, the magnesium oxide is good in high-temperature stability and can stably exist in a binary system of fused salt, and compared with magnesium oxide powder, the magnesium oxide fiber reduces the using amount of magnesium oxide while ensuring the conductivity of a sample due to the fact that the fiber forms a net structure extending in three spatial directions, so that the thermal battery is smaller in volume and higher in electricity storage efficiency. To achieve such an object, the magnesium oxide fibers now exhibit good flow-inhibiting ability and ability to improve electrical properties of the electrolyte sheet, and better development in terms of flow-inhibiting and electrical properties improvement is fully possible.
In addition, the high-activity magnesium oxide fiber and the low-activity magnesium oxide fiber are widely applied to the fields of engineering plastics, pharmaceutical chemicals, petrochemical industry, paint, graphite, ceramics, fire resistance and the like, and can also be used as additives of foods and feeds and the like. The activity is higher, the specific surface area is larger, and the molten electrolyte can be better supported. Potassium magnesium sulfate and potassium sulfate are very high-quality fertilizers and are widely used in agricultural production.
Disclosure of Invention
The invention aims to provide a method for jointly producing magnesium oxide fibers and potassium sulfate/magnesium sulfate potash fertilizers, which can produce magnesium sulfate fertilizers or magnesium sulfate potash fertilizers while producing magnesium oxide fibers, does not generate pollutants, and obviously improves the economic benefit of the products.
The purpose of the invention is realized by the following technical scheme:
a method for co-producing magnesium oxide fiber and potassium sulfate/potash fertilizer, the method comprising the steps of: adding polyethylene glycol accounting for 20.0-40.0wt% of the mass of the magnesium sulfate into a magnesium sulfate solution, uniformly stirring a heptahydrate magnesium sulfate solution mixed with the polyethylene glycol, and then adding a mixture of anhydrous potassium carbonate and the magnesium sulfate according to a molar ratio of 1: 1-1.2, slowly dripping a potassium carbonate solution into the magnesium sulfate mixed solution at room temperature, stirring for 20-60min after completion, aging for two hours, filtering a reactant, wherein a filtrate is a potassium sulfate fertilizer or a magnesium sulfate potassium fertilizer, a precipitate is a precursor of magnesium oxide fibers, and calcining the washed and dried precursor to a certain temperature to prepare the magnesium oxide fibers.
The method for jointly producing the magnesium oxide fiber and the potassium sulfate/magnesium sulfate potash fertilizer comprises the steps of heating a precursor to 550-800 ℃ to prepare the high-activity magnesium oxide fiber; heating the precursor to 1600 ℃ to prepare the low-activity magnesium oxide fiber.
The invention has the advantages and positive effects that:
in the process of preparing the magnesium oxide fiber, the potassium sulfate fertilizer or the magnesium sulfate potash fertilizer is produced, no industrial waste and pollutant are generated, and the economic benefit of the product is obviously improved.
Drawings
FIG. 1 is an SEM picture of MgO fiber prepared by calcination at 1550 ℃ in example of the present invention;
FIG. 2 is an SEM picture of MgO fiber obtained by calcination at 800 ℃ in example of the present invention;
FIG. 3 is an SEM photograph of MgO fibers obtained by calcination at 600 ℃ in example of the present invention;
FIG. 4 is an SEM photograph of MgO fibers obtained by calcination at 1600 ℃ in example of the present invention.
Detailed Description
The present invention will be described in detail with reference to the embodiments shown in the drawings.
Example 1
The method comprises the following steps:
adding polyethylene glycol accounting for 20.0wt% of the mass of magnesium sulfate into a magnesium sulfate solution, uniformly stirring a heptahydrate magnesium sulfate solution mixed with the polyethylene glycol, and then adding a mixture of anhydrous potassium carbonate and magnesium sulfate according to a molar ratio of 1: 1, slowly dripping a potassium carbonate solution into the magnesium sulfate mixed solution at room temperature, stirring for 60min after completion, aging for two hours, filtering reactants, calcining the washed and dried precursors to the temperature of 550-800 ℃, and preparing the high-activity magnesium oxide fiber, wherein the filtrate is a potassium sulfate fertilizer, and the precipitate is a precursor of the magnesium oxide fiber.
The result of the detection
SEM picture of MgO fiber prepared by calcination at 1550 ℃;
SEM picture of MgO fiber prepared by calcination at 2800 ℃.
As can be seen from fig. 1 and 2: the length of the magnesium oxide fiber prepared by the method is 3-15 microns, the dispersion is good, but the magnesium oxide fiber prepared at 800 ℃ has partial agglomeration.
The activities of MgO fibers prepared by calcining at 550 ℃ and 800 ℃ are 89.0 percent and 87.6 percent respectively.
The content of potassium sulfate in the filtrate is 30.5%, and the filtrate can be directly used for agricultural production or used for extracting solid potassium sulfate after evaporating the solution.
Example 2
The method comprises the following steps:
adding polyethylene glycol accounting for 40.0wt% of the mass of the magnesium sulfate into a magnesium sulfate solution, uniformly stirring a heptahydrate magnesium sulfate solution mixed with the polyethylene glycol, and then adding a mixture of anhydrous potassium carbonate and the magnesium sulfate according to a molar ratio of 1: 1.1, slowly dropwise adding a potassium carbonate solution into the magnesium sulfate mixed solution at room temperature, stirring for 60min after completion, aging for two hours, filtering the reactant, wherein the filtrate is a magnesium sulfate potash fertilizer, the precipitate is a precursor of magnesium oxide fibers, filtering the reactant, the filtrate is a potassium sulfate fertilizer, the precipitate is a precursor of magnesium oxide fibers, calcining the washed and dried precursor to 700 ℃, and preparing the high-activity magnesium oxide fibers.
And (3) detection results:
as shown in SEM picture of MgO fiber prepared by calcining at 3600 ℃;
as can be seen in fig. 3: the length of the magnesium oxide fiber prepared by the method is 10-50 microns, the dispersion is good, but the magnesium oxide fiber prepared at 600 ℃ is partially agglomerated.
The activities of the MgO fibers prepared by calcining at 600 ℃ are respectively 90.3 percent, and the activity is better. The content of the magnesium sulfate and the potassium sulfate in the filtrate is 30.5 percent, and the filtrate can be directly used for agricultural production or used for extracting solid magnesium sulfate and potassium after solution evaporation.
Example 3
The method comprises the following steps:
adding polyethylene glycol accounting for 30.0wt% of the mass of magnesium sulfate into a magnesium sulfate solution, uniformly stirring a heptahydrate magnesium sulfate solution mixed with the polyethylene glycol, and then adding a mixture of anhydrous potassium carbonate and magnesium sulfate according to a molar ratio of 1: 1.2, slowly dropwise adding a potassium carbonate solution into the magnesium sulfate mixed solution at room temperature, stirring for 60min after completion, aging for two hours, filtering the reactant, wherein the filtrate is a magnesium sulfate potash fertilizer, the precipitate is a precursor of magnesium oxide fibers, filtering the reactant, the filtrate is a potassium sulfate fertilizer, the precipitate is a precursor of magnesium oxide fibers, calcining the washed and dried precursor to 1600 ℃, and preparing the low-activity magnesium oxide fibers.
And (3) detection results:
as shown in the SEM picture of MgO fiber prepared by calcination at 41600 ℃;
as can be seen in fig. 4: the magnesium oxide fiber prepared by the method has the length of 10-50 microns and good dispersion, but the magnesium oxide fiber prepared at 1600 ℃ has part.
The activities of the MgO fibers prepared by calcining at 1600 ℃ are respectively 0.6 percent. The content of the magnesium sulfate and the potassium sulfate in the filtrate is 32.8 percent, and the filtrate can be directly used for agricultural production or used for extracting solid magnesium sulfate and potassium after solution evaporation.
Claims (2)
1. A method for the joint production of magnesium oxide fibre and potassium sulphate/sulphate-potassium fertilizer, characterised in that the method comprises the steps of: adding polyethylene glycol accounting for 20.0-40.0wt% of the mass of the magnesium sulfate into a magnesium sulfate solution, uniformly stirring a heptahydrate magnesium sulfate solution mixed with the polyethylene glycol, and then adding a mixture of anhydrous potassium carbonate and the magnesium sulfate according to a molar ratio of 1: 1-1.2, slowly dripping a potassium carbonate solution into the magnesium sulfate mixed solution at room temperature, stirring for 20-60min after completion, aging for two hours, filtering a reactant, wherein a filtrate is a potassium sulfate fertilizer or a magnesium sulfate potassium fertilizer, a precipitate is a precursor of magnesium oxide fibers, and calcining the washed and dried precursor to a certain temperature to prepare the magnesium oxide fibers.
2. The method for the combined production of magnesium oxide fiber and potassium sulfate/potash fertilizer as claimed in claim 1, wherein the precursor is heated to 550-800 ℃ to prepare the high-activity magnesium oxide fiber; heating the precursor to 1600 ℃ to prepare the low-activity magnesium oxide fiber.
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CN202010999811.2A CN112159254A (en) | 2020-09-22 | 2020-09-22 | Method for joint production of magnesium oxide fiber and potassium sulfate/magnesium sulfate potash fertilizer |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103204524A (en) * | 2013-04-08 | 2013-07-17 | 西南科技大学 | Preparation method of magnesium oxide porous fiber |
CN103274434A (en) * | 2013-05-07 | 2013-09-04 | 中国恩菲工程技术有限公司 | Method for recycling magnesium ions from magnesium sulfate solution |
CN104529487A (en) * | 2014-12-15 | 2015-04-22 | 山东大学 | Ultrahigh-temperature magnesium oxide fibre product and preparation method thereof |
CN105489910A (en) * | 2015-07-31 | 2016-04-13 | 西南科技大学 | Preparation method of electrolyte flake for thermal battery |
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2020
- 2020-09-22 CN CN202010999811.2A patent/CN112159254A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103204524A (en) * | 2013-04-08 | 2013-07-17 | 西南科技大学 | Preparation method of magnesium oxide porous fiber |
CN103274434A (en) * | 2013-05-07 | 2013-09-04 | 中国恩菲工程技术有限公司 | Method for recycling magnesium ions from magnesium sulfate solution |
CN104529487A (en) * | 2014-12-15 | 2015-04-22 | 山东大学 | Ultrahigh-temperature magnesium oxide fibre product and preparation method thereof |
CN105489910A (en) * | 2015-07-31 | 2016-04-13 | 西南科技大学 | Preparation method of electrolyte flake for thermal battery |
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