CN116835618A - Synthesis method of magnesium nitrate hexahydrate based on microcrystalline magnesite - Google Patents
Synthesis method of magnesium nitrate hexahydrate based on microcrystalline magnesite Download PDFInfo
- Publication number
- CN116835618A CN116835618A CN202310675179.XA CN202310675179A CN116835618A CN 116835618 A CN116835618 A CN 116835618A CN 202310675179 A CN202310675179 A CN 202310675179A CN 116835618 A CN116835618 A CN 116835618A
- Authority
- CN
- China
- Prior art keywords
- microcrystalline
- magnesite
- magnesium nitrate
- nitrate hexahydrate
- magnesium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 title claims abstract description 88
- 239000001095 magnesium carbonate Substances 0.000 title claims abstract description 88
- 229910000021 magnesium carbonate Inorganic materials 0.000 title claims abstract description 88
- 235000014380 magnesium carbonate Nutrition 0.000 title claims abstract description 88
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 238000001308 synthesis method Methods 0.000 title claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000011777 magnesium Substances 0.000 claims abstract description 25
- 239000002002 slurry Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000001704 evaporation Methods 0.000 claims abstract description 15
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 12
- 238000000967 suction filtration Methods 0.000 claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 28
- 239000000395 magnesium oxide Substances 0.000 claims description 19
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims description 12
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims 6
- 239000006228 supernatant Substances 0.000 claims 3
- 238000006243 chemical reaction Methods 0.000 abstract description 21
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 abstract description 20
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052749 magnesium Inorganic materials 0.000 abstract description 14
- 239000000706 filtrate Substances 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000002253 acid Substances 0.000 abstract description 6
- 238000001556 precipitation Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000003513 alkali Substances 0.000 abstract description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 4
- 235000010755 mineral Nutrition 0.000 abstract description 4
- 239000011707 mineral Substances 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 3
- 230000007062 hydrolysis Effects 0.000 abstract 1
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 14
- 239000002994 raw material Substances 0.000 description 13
- 238000002386 leaching Methods 0.000 description 12
- 239000011575 calcium Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 7
- 229910017604 nitric acid Inorganic materials 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000013081 microcrystal Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 238000007605 air drying Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000012024 dehydrating agents Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000004683 dihydrates Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- -1 fireworks Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000004687 hexahydrates Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- YISKQXFNIWWETM-UHFFFAOYSA-N magnesium;dinitrate;hydrate Chemical compound O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YISKQXFNIWWETM-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004682 monohydrates Chemical class 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- C01F5/38—Magnesium nitrates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a synthesis method of magnesium nitrate hexahydrate based on microcrystalline magnesite, and belongs to the technical field of mineral processing. The synthesis method comprises the following steps: firstly, crushing microcrystalline magnesite, and then performing washing ball milling to obtain microcrystalline magnesite powder; dispersing the ball-milled microcrystalline magnesite powder into water to form slurry, and carrying out suction filtration after hydrolysis and precipitation reaction; and (3) centrifugally separating the filtrate obtained after suction filtration to obtain a magnesium nitrate solution, evaporating and concentrating at 60-80 ℃, and cooling and crystallizing to obtain magnesium nitrate hexahydrate. The method directly takes the microcrystalline magnesite raw ore as a magnesium source, and the reaction process is hydrolysis reaction without the participation of strong acid and strong alkali. The preparation method is safe, nontoxic, green and environment-friendly, simplifies the production process of the magnesium nitrate hexahydrate, and reduces the cost for preparing the magnesium nitrate hexahydrate.
Description
Technical Field
The invention belongs to the technical field of mineral processing, and particularly relates to a method for preparing magnesium nitrate hexahydrate by directly leaching magnesium element from microcrystalline magnesite serving as a raw material.
Background
China has rich magnesite mineral resources and huge reserves. The natural magnesite is mainly divided into crystalline magnesite and microcrystalline magnesite, and the crystalline magnesite is mainly developed and used at present. The production of magnesia raw materials such as sintered magnesia, fused magnesia, light burned magnesia and the like which are processed by magnesite every year is the first place in the world. The Tibetan kamaduo magnesite is only one high-grade large-sized microcrystalline magnesite which is known to exist in terrestrial magnesite worldwide, and the high-quality product ore accounts for 90% of the total reserve. The light burned magnesia obtained by calcining the microcrystalline magnesite at high temperature has higher purity, and the magnesia content can reach 98.79 percent. Compared with magnesite in northeast China, the microcrystalline magnesite has lower content of impurity elements such as iron, aluminum, silicon, calcium and the like. And the problem that the magnesium source obtained after seawater concentration and extraction contains chlorine is avoided. Therefore, the Tibetan microcrystal magnesite is very suitable for being used as a production environment-friendly high-end magnesia chemical raw material. According to the characteristics, the microcrystalline magnesite can produce magnesium nitrate hexahydrate with better quality at low cost.
Magnesium nitrate is an inorganic compound with the chemical formula of Mg (NO 3 ) 2 Is white crystalline powder, and is dissolved in water, methanol, ethanol, and liquid ammonia, and the aqueous solution is neutral, and can be used as dehydrating agent, catalyst, wheat ashing agent, and analytical test for concentrated nitric acidAgents, and the preparation of magnesium salts, and the like. Magnesium nitrate hydrate is usually present in the form of monohydrate, dihydrate, or hexahydrate. However, magnesium nitrate hexahydrate is mostly sold in the market and is often used as a dehydrating agent for concentrating nitric acid to prepare explosives, fireworks, raw materials for preparing catalysts, strong oxidants and other nitrates.
At present, two main preparation modes of magnesium nitrate exist: magnesium oxide and magnesium carbonate processes. The magnesia process is to add light magnesia into 30-50% concentration dilute nitric acid solution and react while stirring slowly until the solution is neutral. The reaction temperature is kept below 60 ℃. Evaporating and concentrating the reaction solution, cooling and crystallizing, centrifugally separating, and air-drying to obtain the magnesium nitrate finished product. The reaction equation is: mgO+2HNO 3 →Mg(NO 3 ) 2 +H 2 O. The magnesium carbonate method is to slowly add excessive magnesite powder (MgCO) into 35% -40% dilute nitric acid solution 3 ). The carbon dioxide gas released from the reaction causes foaming of the solution, and the reaction solution is heated to 105-115 ℃ due to the heat of reaction, thereby promoting nitric acid loss and keeping the reaction temperature at 40-50 ℃. And (3) reacting until the pH value of the solution reaches 4-5, filtering, evaporating, concentrating, cooling, crystallizing, centrifugally separating, and air-drying to obtain a magnesium nitrate finished product. The reaction equation is: mgCO 3 +2HNO 3 →Mg(NO 3 ) 2 +H 2 O+CO 2 And ≡. At present, magnesium nitrate is produced by using magnesium oxide and nitric acid as raw materials. Chinese patent (CN 106517266A) discloses a method for producing magnesium nitrate hexahydrate by taking magnesium oxide and dilute nitric acid as raw materials, which comprises the specific processes of adding the magnesium oxide into a reaction kettle filled with the dilute nitric acid in proportion for reaction, controlling the temperature and the pH value of the reaction kettle, carrying out solid-liquid separation on reaction liquid, filtering inorganic impurities, directly feeding filtrate into a storage tank with heat preservation, and carrying out a granulating process to obtain a granular magnesium nitrate finished product. The magnesium nitrate is synthesized by the traditional method, and the microcrystalline magnesite is calcined and decomposed under the high temperature condition to generate magnesium oxide, and then the magnesium nitrate hexahydrate is obtained by acid leaching reaction. The calcination process has strict technological requirements and consumes a large amount of energy, which is unfavorable for energy conservation and emission reduction. In addition, acid leachingThe use of Cheng Jiangsuan strong alkali can cause certain harm to the environment and the health of human bodies. Therefore, developing a technology that can directly leach magnesium element in microcrystalline magnesite ore without calcining and acid leaching processes is a key for future development of the mineral processing industry.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing magnesium nitrate hexahydrate by directly leaching magnesium element from microcrystalline magnesite. The method has the advantages of simple production process, environmental protection, no participation of acid-base solution in the reaction process, and improved economic and environmental protection benefits. In order to solve the problems of complex operation, long production period and the like in the production process, the production method of magnesium nitrate hexahydrate is simple to operate, low in equipment investment and short in production period.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the synthesis method of magnesium nitrate hexahydrate based on microcrystalline magnesite uses raw microcrystalline magnesite as raw material, and directly uses magnesium element to leach out to prepare magnesium nitrate hexahydrate. The method not only avoids high-temperature calcination of the microcrystalline magnesite, reduces energy consumption, but also gets rid of dependence of the reaction process on strong acid and strong alkali, and is healthy and environment-friendly. The method comprises the following specific steps:
(1) Pretreatment of microcrystalline magnesite: firstly crushing microcrystalline magnesite, and performing washing ball milling to obtain microcrystalline magnesite powder;
(2) Hydrolysis reaction: dispersing the ball-milled microcrystalline magnesite powder into water to form slurry, adding ferric nitrate nonahydrate into the slurry, and carrying out suction filtration after hydrolysis reaction;
(3) Evaporating and concentrating, cooling and crystallizing: evaporating and concentrating the magnesium nitrate solution obtained by suction filtration at 60-80 ℃, and cooling and crystallizing to obtain magnesium nitrate hexahydrate.
According to the invention, the magnesium oxide content of the microcrystalline magnesite ore described in step (1) is 47.5-47.8%.
According to the invention, the microcrystalline magnesite in the step (1) is crushed and ball-milled to obtain microcrystalline magnesite micro powder with the particle size of 2-5 mu m.
According to the invention, the mass ratio of the microcrystalline magnesite powder to the water added in the slurry in the step (2) is 1:10-1:40.
According to the invention, ca in the microcrystalline magnesite powder added in the filtrate in the step (2) 2+ With Mg 2+ The ratio of the sum of the amounts of the substances of (2) to the amount of the substance of ferric nitrate nonahydrate is 2-4:1-2.
According to the invention, the hydrolysis reaction temperature in the step (2) is 50-70 ℃, the reaction time is 2-4h, and the stirring rotation speed is 200-400 r/min.
According to the invention, the magnesium nitrate solution obtained by suction filtration in the step (3) is evaporated and concentrated for 3 to 5 hours at the temperature of 60 to 80 ℃.
According to the invention, in step (3), the magnesium nitrate hexahydrate is obtained by cooling crystallization at room temperature.
The related chemical reaction equation for preparing magnesium nitrate hexahydrate by directly leaching magnesium element based on microcrystalline magnesite as a raw material is as follows:
3MgCO 3 +2Fe(NO 3 ) 3 +3H 2 O＝2Fe(OH) 3 ↓+3Mg(NO 3 ) 2 +3CO 2 ↑。
3CaCO 3 +2Fe(NO 3 ) 3 +3H 2 O＝2Fe(OH) 3 ↓+3Ca(NO 3 ) 2 +3CO 2 ↑。
MgCO 3 +Ca(NO 3 ) 2 ＝Mg(NO 3 ) 2 +CaCO 3 ↓。
compared with the prior art, the invention has the beneficial effects that:
magnesium nitrate hexahydrate is prepared by directly leaching magnesium element from microcrystalline magnesite ore as a raw material, has low impurity content, and does not need high-temperature calcination treatment on microcrystalline magnesite. The whole preparation process has simple process flow and does not need the participation of strong acid and strong alkali, thereby being beneficial to improving economic benefit and improving environmental problems. In addition, the preparation of magnesium nitrate hexahydrate by direct magnesium element leaching based on microcrystalline magnesite as a raw material has the characteristics of low cost and high benefit, and is easy to realize industrial production.
Drawings
FIG. 1 is a flow chart of a process for preparing high-purity magnesium nitrate hexahydrate by directly leaching magnesium element in magnesite according to the present invention;
fig. 2 is an XRD spectrum of magnesium nitrate hexahydrate prepared in example 1.
Detailed Description
The technical scheme and effect of the present invention will be further described with reference to specific examples, but the scope of the present invention is not limited thereto.
Example 1
A method for preparing magnesium nitrate hexahydrate by directly leaching magnesium element based on microcrystalline magnesite as a raw material is shown in figure 1, and comprises the following steps:
pretreatment of microcrystalline magnesite: placing the raw microcrystalline magnesite ore with the magnesium oxide content of 47.5-47.8% into a jaw crusher for crushing, and then washing with water and performing ball milling treatment to obtain microcrystalline magnesite powder with the average particle size of 2-5 mu m;
preparing slurry: dispersing the treated microcrystalline magnesite powder into distilled water according to the mass ratio of the microcrystalline magnesite powder to water of 1:10 to form slurry;
hydrolysis reaction: according to Ca in microcrystal magnesite powder 2+ With Mg 2+ Adding ferric nitrate nonahydrate into the slurry according to the mass ratio of the sum of the substances to the ferric nitrate nonahydrate of 3:2, then placing the slurry on a constant-temperature magnetic stirrer, continuously stirring for 2 hours under the conditions of 50 ℃ and 200r/min of rotating speed, and then carrying out suction filtration to obtain filtrate;
and (3) evaporating and concentrating: evaporating and concentrating the filtrate obtained after the precipitation reaction for 4 hours at 70 ℃, and stopping heating when a crystal film appears on the upper layer of the solution;
cooling and crystallizing: cooling and crystallizing at room temperature to obtain magnesium nitrate hexahydrate crystal.
The XRD patterns of the magnesium nitrate hexahydrate obtained in this example are shown in FIG. 1, and the diffraction peaks of the magnesium nitrate hexahydrate are consistent with the data corresponding to the pdf (14-0101) card of the standard magnesium nitrate hexahydrate. The magnesium nitrate hexahydrate prepared by the method has higher purity and good crystallinity.
Example 2
A method for preparing magnesium nitrate hexahydrate by directly leaching magnesium element based on microcrystalline magnesite as a raw material is shown in figure 1, and comprises the following steps:
pretreatment of microcrystalline magnesite: placing the raw microcrystalline magnesite ore with the magnesium oxide content of 47.5-47.8% into a jaw crusher for crushing, and then washing with water and performing ball milling treatment to obtain microcrystalline magnesite powder with the average particle size of 2-5 mu m;
preparing slurry: dispersing the treated microcrystalline magnesite powder into distilled water according to the mass ratio of the microcrystalline magnesite powder to water of 1:10 to form slurry;
hydrolysis reaction: according to Ca in microcrystal magnesite powder 2+ With Mg 2+ Adding ferric nitrate nonahydrate into the slurry according to the mass ratio of the sum of substances and the ferric nitrate nonahydrate of 2:1, then placing the slurry on a constant-temperature magnetic stirrer, continuously stirring for 2 hours under the conditions of 50 ℃ and 200r/min of rotating speed, and then carrying out suction filtration to obtain filtrate;
and (3) evaporating and concentrating: evaporating and concentrating the filtrate obtained after the precipitation reaction at 60 ℃ for 3 hours, and stopping heating when a crystal film appears on the upper layer of the solution;
cooling and crystallizing: cooling and crystallizing at room temperature to obtain magnesium nitrate hexahydrate crystal.
Example 3
A method for preparing magnesium nitrate hexahydrate by directly leaching magnesium element based on microcrystalline magnesite as a raw material is shown in figure 1, and comprises the following steps:
pretreatment of microcrystalline magnesite: placing the raw microcrystalline magnesite ore with the magnesium oxide content of 47.5-47.8% into a jaw crusher for crushing, and then washing with water and performing ball milling treatment to obtain microcrystalline magnesite powder with the average particle size of 2-5 mu m;
preparing slurry: dispersing the treated microcrystalline magnesite powder into distilled water according to the mass ratio of the microcrystalline magnesite powder to water of 1:10 to form slurry;
hydrolysis reaction: according to Ca in microcrystal magnesite powder 2+ With Mg 2+ Adding ferric nitrate nonahydrate to the slurry in a ratio of 3:1 of the sum of the amounts of the substances of (a) to the amount of ferric nitrate nonahydrate, then placing the mixture on a constant temperature magnetic stirrer at a temperature of 55 ℃,continuously stirring for 2 hours at the rotating speed of 200r/min, and then carrying out suction filtration to obtain filtrate;
and (3) evaporating and concentrating: evaporating and concentrating the filtrate obtained after the precipitation reaction for 4 hours at 70 ℃, and stopping heating when a crystal film appears on the upper layer of the solution;
cooling and crystallizing: cooling and crystallizing at room temperature to obtain magnesium nitrate hexahydrate crystal.
Example 4
A method for preparing magnesium nitrate hexahydrate by directly leaching magnesium element based on microcrystalline magnesite as a raw material is shown in figure 1, and comprises the following steps:
pretreatment of microcrystalline magnesite: placing the raw microcrystalline magnesite ore with the magnesium oxide content of 47.5-47.8% into a jaw crusher for crushing, and then washing with water and performing ball milling treatment to obtain microcrystalline magnesite powder with the average particle size of 2-5 mu m;
preparing slurry: dispersing the treated microcrystalline magnesite powder into distilled water according to the mass ratio of the microcrystalline magnesite powder to water of 1:10 to form slurry;
hydrolysis reaction: according to Ca in microcrystal magnesite powder 2+ With Mg 2+ Adding ferric nitrate nonahydrate into the slurry according to the mass ratio of the sum of substances and the ferric nitrate nonahydrate of 4:1, then placing the slurry on a constant-temperature magnetic stirrer, continuously stirring for 3 hours under the conditions of 60 ℃ and the rotating speed of 300r/min, and then carrying out suction filtration to obtain filtrate;
and (3) evaporating and concentrating: evaporating and concentrating the filtrate obtained after the precipitation reaction at 80 ℃ for 5 hours, and stopping heating when a crystal film appears on the upper layer of the solution;
cooling and crystallizing: cooling and crystallizing at room temperature to obtain magnesium nitrate hexahydrate crystal.
TABLE 1 chemical index of magnesium nitrate hexahydrate prepared in examples 1-4
| Index (I) | Example 1 | Example 2 | Example 3 | Example 4 |
| Content (Mg (NO) 3 ) 2 ·6H 2 O)/％ | 99.5 | 99.0 | 99.2 | 99.3 |
| Water insoluble/% | 0.015 | 0.020 | 0.016 | 0.018 |
| Chloride (Cl)/% | 0.005 | 0.008 | 0.006 | 0.006 |
| Sulfate (SO) 4 )/％ | 0.014 | 0.016 | 0.015 | 0.016 |
| Calcium (Ca)/% | 0.010 | 0.030 | 0.020 | 0.030 |
| Iron (Fe)/% | 0.001 | 0.002 | 0.004 | 0.001 |
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A synthesis method of magnesium nitrate hexahydrate based on microcrystalline magnesite, which is characterized by comprising the following steps:
(1) Pretreatment of microcrystalline magnesite: crushing microcrystalline magnesite, and then washing and ball milling to obtain microcrystalline magnesite powder;
(2) Hydrolysis reaction: dispersing microcrystalline magnesite powder into water to form slurry, adding ferric nitrate nonahydrate into the slurry, carrying out hydrolysis reaction, and carrying out suction filtration to obtain supernatant;
(3) Evaporating and concentrating, cooling and crystallizing: evaporating and concentrating the supernatant obtained by suction filtration at 50-80 ℃, and cooling and crystallizing to obtain magnesium nitrate hexahydrate.
2. The method for synthesizing magnesium nitrate hexahydrate based on microcrystalline magnesite according to claim 1, wherein the magnesium oxide content in the microcrystalline magnesite in step (1) is 47.5-47.8%.
3. The method for synthesizing magnesium nitrate hexahydrate based on microcrystalline magnesite according to claim 1, wherein the average grain size of the microcrystalline magnesite powder in the step (1) is 2 to 5 μm.
4. The method for synthesizing magnesium nitrate hexahydrate based on microcrystalline magnesite according to claim 1, wherein the mass ratio of microcrystalline magnesite powder to water in the slurry in the step (2) is 1:10-1:40.
5. The method for synthesizing magnesium nitrate hexahydrate based on microcrystalline magnesite according to claim 1, wherein the microcrystalline magnesite powder Ca in the slurry in the step (2) 2+ With Mg 2+ The ratio of the sum of the amounts of the substances of (2) to the amount of the substance of ferric nitrate nonahydrate is 2-4:1-2.
6. The method for synthesizing magnesium nitrate hexahydrate based on microcrystalline magnesite according to claim 1, wherein the hydrolysis reaction temperature in the step (2) is 50-70 ℃, the reaction time is 2-4 hours, and the stirring rotation speed is 200-400 r/min.
7. The method for synthesizing magnesium nitrate hexahydrate based on microcrystalline magnesite according to claim 1, wherein the supernatant obtained by suction filtration in the step (3) is evaporated and concentrated for 3-5 hours, and then cooled and crystallized at room temperature to obtain magnesium nitrate hexahydrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310675179.XA CN116835618A (en) | 2023-06-08 | 2023-06-08 | Synthesis method of magnesium nitrate hexahydrate based on microcrystalline magnesite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310675179.XA CN116835618A (en) | 2023-06-08 | 2023-06-08 | Synthesis method of magnesium nitrate hexahydrate based on microcrystalline magnesite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116835618A true CN116835618A (en) | 2023-10-03 |
Family
ID=88166140
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310675179.XA Pending CN116835618A (en) | 2023-06-08 | 2023-06-08 | Synthesis method of magnesium nitrate hexahydrate based on microcrystalline magnesite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116835618A (en) |
-
2023
- 2023-06-08 CN CN202310675179.XA patent/CN116835618A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2010088863A1 (en) | Method for depositing metal ions | |
| US7771682B2 (en) | Process for the preparation of magnesia (MgO) from crude Mg (OH)2 | |
| CN101607720A (en) | With the bittern that contains magnesium chloride is the feedstock production method of magnesium oxide | |
| CN110699756B (en) | Method for preparing alpha-type gypsum whisker by using ammonia-soda waste liquid | |
| Yu et al. | Preparation of crystalline mixed rare earth carbonates by Mg (HCO3) 2 precipitation method | |
| CN102126734A (en) | Process for removing calcium from magnesite | |
| CN102502722A (en) | Preparation method of high-purity magnesium oxide | |
| CN101804998B (en) | Method for producing high-purity magnesium oxide by using dolomite | |
| CN109437261A (en) | A kind of sheeted nanometer magnesium hydroxide raw powder's production technology | |
| CN107032384B (en) | A method of separating and recovering calcium and magnesium from Calcium magnesium minerals | |
| CN111825111A (en) | Preparation method for improving thermal stability of magnesium-aluminum hydrotalcite | |
| CN104968605B (en) | Magnesite prepares the method for lamellar dispersed nano magnesium hydroxide | |
| CN102424409B (en) | Method for preparing light magnesium carbonate | |
| CN102703982A (en) | Method for preparing magnesium carbonate trihydrate crystal whisker by utilizing serpentine | |
| CN101374767B (en) | An improved process for preparation of magnesium oxide | |
| CN100363262C (en) | Method for producing alumina | |
| CN115353139B (en) | Preparation method of high-purity calcium carbonate | |
| CN102838141A (en) | Process for producing magnesium hydrate by removing silicon and aluminum from magnesite | |
| CN104803400A (en) | Ammonium magnesium sulfate preparation method | |
| CN116835618A (en) | Synthesis method of magnesium nitrate hexahydrate based on microcrystalline magnesite | |
| CN115072749B (en) | Method for extracting lithium from spodumene without slag | |
| CN1868952A (en) | Method of producing magnesium hydroxide and light magnesium oxide using magnesite as raw material | |
| CN102115813B (en) | Comprehensive utilization method for low-grade magnesite | |
| CN109354048B (en) | Method for preparing magnesium hydroxide and magnesium carbonate series compound by ion catalysis of magnesite | |
| CN101774614A (en) | Preparation method of magnesium oxide by using bittern and carbonate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |