CN104724735A - Method for preparing anhydrous magnesium carbonate powder by solvothermal method - Google Patents
Method for preparing anhydrous magnesium carbonate powder by solvothermal method Download PDFInfo
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- CN104724735A CN104724735A CN201510078278.5A CN201510078278A CN104724735A CN 104724735 A CN104724735 A CN 104724735A CN 201510078278 A CN201510078278 A CN 201510078278A CN 104724735 A CN104724735 A CN 104724735A
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- anhydrous magnesium
- carbonate powder
- magnesium carbonate
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- 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
- C01F5/24—Magnesium carbonates
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- 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
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- 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 discloses a method for preparing anhydrous magnesium carbonate powder by a solvothermal method. The method comprises the steps of mixing soluble magnesium salt and soluble carbonate in a molar ratio of 1: (1-1.5), controlling the reaction temperature to 100-200 DEG C in a solvothermal system, performing autoclave solvothermal reaction for 3-24 hours while stirring, cooling, filtering the obtained white sediment, washing, drying and crushing to obtain the single-phase anhydrous magnesium carbonate powder. The method is reasonable in process, facilitates industrialized enlarged production, and is low in cost; the product is wide in application field, large in market potential and strong in competitiveness; and the method has significant economical and social benefits, and has novelty and innovation.
Description
Technical field
The invention belongs to inorganic chemical industry synthesis field, be specifically related to a kind of solvent thermal and prepare the method for synthesizing single thing phase anhydrous magnesium carbonate powder.
Background technology
Magnesiumcarbonate is a kind of important inorganic chemical industry material, has good fillibility, dispersiveness and flame retardant resistance, is added in engineering plastics, can significantly improve the high temperature resistant of engineering plastics and flame retardant properties.The so-called magnesiumcarbonate product be called for short in the market is all hydrated basic magnesium carbonate mostly except magnisite magnesiumcarbonate.
The anhydrous magnesium carbonate preparing single thing phase is a challenge for chemist always, the good news is the continuous effort through vast researcher, propose some useful preparation methods, prepare the method for magnesiumcarbonate in a kind of circulatory mediator as professor's Shen Xing report in patent CN1362371A, report a kind of hydrothermal method in patent CN102153115A and utilize the method that magnesium chloride and urea are Material synthesis single thing phase magnesiumcarbonate.Also has in patent CN1854068A a kind of method that have recorded supercutical fluid and prepare magnesiumcarbonate.
Under the condition of the aqueous solution, the difficult point preparing single thing phase magnesiumcarbonate is that the solubleness of magnesium hydroxide is also less than magnesiumcarbonate, thus very easily forms symbiosis precipitation, generates hydrated basic magnesium carbonate.Based on above-mentioned analysis, under therefore the present invention proposes solvent thermal condition, synthesize the method for single-phase anhydrous magnesium carbonate.
Summary of the invention
The preparation method of the anhydrous magnesium carbonate powder of single thing phase, for raw material with solubility magnesium salts and soluble carbonate salt, the ratio of 1:1 ~ 1.5 in molar ratio, in the system of solvent thermal, controls temperature of reaction at 100-200 DEG C, under agitation carry out autoclave solvent thermal reaction 3-24 hour, cooling, filters the white precipitate of gained, washing, drying and pulverizing, obtain the anhydrous magnesium carbonate powder of single thing phase.
Performance test is carried out to the white powder of gained, measures crystalline phase with X-ray diffractometer, by pattern and the size of scanning electron microscopy measurement powder.
Through the anhydrous magnesium carbonate that described scheme is synthesized, as can be seen from attached X-ray diffractogram illustrated in Figure 1 (XRD): this spectrogram and anhydrous magnesium carbonate standard spectrogram JCPDS No. 8-479 completely the same, not there is impurity peaks, main peak is sharp-pointed, illustrate that product purity is very high, and crystallization is complete, is six side's calcite crystal formations.The SEM photo of attached this product illustrated in Figure 2, uniform particles and favorable dispersity, particle diameter concentrates on 1-2 μm.
Compared with prior art, advantage of the present invention shows: ensure that single thing phase under utilizing solvent thermal condition, and the raw material used is easy to get and cheap, the remarkable advantages such as product good dispersion property.Present method processing requirement is simple, and production process is easy to control, is easy to amplification and carries out suitability for industrialized production.Present invention process is reasonable, with low cost, and product applications is extensive, and market potential is large, and competitive power is strong, has significant economic and social benefit, has novelty and novelty.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction pattern of the anhydrous magnesium carbonate of embodiment 1 gained.
Fig. 2 is the microscopic appearance SEM photo of the anhydrous magnesium carbonate of embodiment 1 gained.
Embodiment
Content of the present invention can be further illustrated with example below, only illustrate for being used for and embodying processing method of the present invention, instead of limiting the scope of the invention and application places.To those skilled in the art, obviously when use distinct device and usual available raw material are implemented of the present invention, new modification can be introduced, but such modification can not be thought beyond by the determined scope of the present invention of claims.
Embodiment 1:
Take the magnesium sulfate of 1mol and the sodium carbonate of 1.2mol, join in autoclave, add quadrol solvent to autoclave body long-pending 80%, open stirring, sealing, be heated to 180 DEG C, keep 6 hours, Temperature fall, by the white precipitate washing obtained, filter cake will be obtained be placed in 80 DEG C, baking oven and dry, pulverize, obtain white powder.The interpretation of result of product as shown in Figures 1 and 2.
Embodiment 2:
Take the magnesium chloride of 1mol and the sodium carbonate of 1.2mol, join in autoclave, add tetrahydrofuran solvent to autoclave body long-pending 80%, open stirring, sealing, be heated to 130 DEG C, keep 20 hours, Temperature fall, by the white precipitate washing obtained, filter cake will be obtained be placed in 80 DEG C, baking oven and dry, pulverize, obtain white powder.
Embodiment 3:
Take the magnesium nitrate of 1mol and the salt of wormwood of 1.2mol, join in autoclave, add solvent dimethylformamide to autoclave body long-pending 80%, open stirring, sealing, be heated to 150 DEG C, keep 24 hours, Temperature fall, by the white precipitate washing obtained, filter cake will be obtained be placed in 80 DEG C, baking oven and dry, pulverize, obtain white powder.
Embodiment 4:
Take the magnesium acetate of 1mol and the volatile salt of 1.3mol, join in autoclave, add anhydrous ethanol solvent to autoclave body long-pending 80%, open stirring, sealing, be heated to 180 DEG C, keep 10 hours, Temperature fall, by the white precipitate washing obtained, filter cake will be obtained be placed in 80 DEG C, baking oven and dry, pulverize, obtain white powder.
Compared with more current preparation methods, the present invention has raw material and is easy to get, and processing requirement is simple, the remarkable advantages such as production process is easy to control, and product good dispersion property, manufacturing cost are low.The powder of preparation can substitute magnesium hydroxide completely as fire retardant, for PVC, EVA isoelectric line cable, and the polyolefin resines such as PP, PE, rubber, the fields such as engineering plastics.
Claims (4)
1. under a solvent thermal condition, the method for the anhydrous magnesium carbonate powder of single thing phase is synthesized in preparation, in turn include the following steps: the ratio of 1:1 ~ 1.5 mixes solubility magnesium salts and soluble carbonate salt in molar ratio, in the system of solvent thermal, control temperature of reaction at 100-200 DEG C, under agitation carry out autoclave solvent thermal reaction 3-24 hour, cooling, the white precipitate of gained is filtered, washing, dry and pulverizing, obtains the anhydrous magnesium carbonate powder of single thing phase.
2. the preparation method of anhydrous magnesium carbonate powder according to claim 1, is characterized in that: described solubility magnesium salts is magnesium chloride, magnesium sulfate, magnesium nitrate or magnesium acetate.
3. the preparation method of anhydrous magnesium carbonate powder according to claim 1, is characterized in that: described soluble carbonate salt is sodium carbonate, salt of wormwood or volatile salt.
4. the preparation method of anhydrous magnesium carbonate powder according to claim 1, is characterized in that: described solvent is quadrol, tetrahydrofuran (THF), dimethyl formamide, methyl alcohol, ethanol, Virahol, acetone, butanone, methyl-2-pyrrolidone, ethyl acetate, butylacetate, ethylene glycol diethyl ether, butyl or propylene glycol monomethyl ether.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510078278.5A CN104724735B (en) | 2015-02-14 | 2015-02-14 | Solvent thermal prepares the method for anhydrous magnesium carbonate powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510078278.5A CN104724735B (en) | 2015-02-14 | 2015-02-14 | Solvent thermal prepares the method for anhydrous magnesium carbonate powder |
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| CN104724735A true CN104724735A (en) | 2015-06-24 |
| CN104724735B CN104724735B (en) | 2016-08-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510078278.5A Expired - Fee Related CN104724735B (en) | 2015-02-14 | 2015-02-14 | Solvent thermal prepares the method for anhydrous magnesium carbonate powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107720790A (en) * | 2017-11-20 | 2018-02-23 | 绵阳市远达新材料有限公司 | The preparation method of heavy magnesium carbonate |
| CN112479237A (en) * | 2020-12-08 | 2021-03-12 | 华东理工大学 | Method for preparing anhydrous magnesium carbonate by directly utilizing salt lake brine |
| CN112794349A (en) * | 2021-01-14 | 2021-05-14 | 江西理工大学 | Method for preparing anhydrous magnesium carbonate by hydrothermal method of large-particle-size magnesium oxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005272752A (en) * | 2004-03-26 | 2005-10-06 | Konoshima Chemical Co Ltd | Anhydrous magnesium carbonate filler, method for producing the same and resin composition |
| CN102153115A (en) * | 2011-05-23 | 2011-08-17 | 大连交通大学 | Method for preparing anhydrous magnesium carbonate powder |
| CN103088400A (en) * | 2012-12-27 | 2013-05-08 | 清华大学 | Method for preparing high-purity magnesium oxide whisker by adopting alcohol-hydrothermal method |
-
2015
- 2015-02-14 CN CN201510078278.5A patent/CN104724735B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005272752A (en) * | 2004-03-26 | 2005-10-06 | Konoshima Chemical Co Ltd | Anhydrous magnesium carbonate filler, method for producing the same and resin composition |
| CN102153115A (en) * | 2011-05-23 | 2011-08-17 | 大连交通大学 | Method for preparing anhydrous magnesium carbonate powder |
| CN103088400A (en) * | 2012-12-27 | 2013-05-08 | 清华大学 | Method for preparing high-purity magnesium oxide whisker by adopting alcohol-hydrothermal method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107720790A (en) * | 2017-11-20 | 2018-02-23 | 绵阳市远达新材料有限公司 | The preparation method of heavy magnesium carbonate |
| CN112479237A (en) * | 2020-12-08 | 2021-03-12 | 华东理工大学 | Method for preparing anhydrous magnesium carbonate by directly utilizing salt lake brine |
| CN112794349A (en) * | 2021-01-14 | 2021-05-14 | 江西理工大学 | Method for preparing anhydrous magnesium carbonate by hydrothermal method of large-particle-size magnesium oxide |
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| CN104724735B (en) | 2016-08-24 |
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