CN101298336A - Synthetic method of magnesium chloride hexammoniate - Google Patents
Synthetic method of magnesium chloride hexammoniate Download PDFInfo
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- CN101298336A CN101298336A CNA2008100624230A CN200810062423A CN101298336A CN 101298336 A CN101298336 A CN 101298336A CN A2008100624230 A CNA2008100624230 A CN A2008100624230A CN 200810062423 A CN200810062423 A CN 200810062423A CN 101298336 A CN101298336 A CN 101298336A
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- magnesium chloride
- magnesium
- ammoniate
- hexammoniate
- hex
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Abstract
The invention discloses a method for synthesizing magnesium chloride hexammoniate. The magnesium silicide and anhydrous ammonium chloride are blended according to the mass ratio of 1:2-1:3, and then lead the two substances to react in the medium of liquid ammonia, and then silane is generated with a large amount of by-product of magnesium chloride hexammoniate. Therefore, compared with other methods, the method can considerably reduce the production cost of magnesium chloride hexammoniate and is beneficial to the circle economy.
Description
Technical field
The present invention relates to a kind of synthesizing magnesium chloride hexammoniate.
Background technology
Magnesium Chloride Anhydrous is the indispensable raw material of electrolytic process production MAGNESIUM METAL, also is the intermediate of numerous catalyzer and medicine.Simultaneously, it also can be used as tackiness agent, frostproofer, peptizer, foodstuff additive etc., is applied to numerous industries such as metallurgy, chemical industry, building and food, has become a kind of important industrial raw material.General metal-salt all contains crystal water, and anhydrous metal salt can be realized by heating hydrated metal salt dehydration method.Magnesium chloride hexahydrate is a kind of modal magnesium chloride hydrate, and chemical formula is MgCl26H2O.Because in the process of heating magnesium chloride hexahydrate, the complex reaction except that dehydration has taken place in it, can not get Magnesium Chloride Anhydrous after the heating.Therefore, the preparation technology of research and development Magnesium Chloride Anhydrous has great importance.
Magnesium chloride hex-ammoniate is the complex compound that Magnesium Chloride Anhydrous and ammonia form, and chemical formula is MgCl
26NH
3All the time, magnesium chloride hex-ammoniate is as a kind of presoma of producing Magnesium Chloride Anhydrous and widespread use.In recent years, the Denmark scientist discovers, magnesium chloride hex-ammoniate has fabulous reversible suction, puts the ammonia characteristic, to obtain hydrogen after the ammonia decomposition, hydrogen-storage amount is up to 9.1%, 6% the standard that surpasses that USDOE proposes, the hydrogen-storage amount that surpasses at present general hydrogen storage material far away is a kind of novel hydrogen storage material that has future.
At present, synthetic magnesium chloride hex-ammoniate mainly contains following three kinds of methods: 1) high boiling solvent system synthesis method, and be about to ammonia and feed the magnesium chloride anhydrous alcohol solution that after dehydration, obtains, generate the magnesium chloride hex-ammoniate precipitation.2) water ammono-system synthesis method will generate magnesium chloride hex-ammoniate in the exsiccant magnesium chloride dihydrate feeding liquefied ammonia.3) low boiling point solvent system synthesis method is utilized low-boiling point alcohol dissolving chlorination magnesium raw material, obtains the magnesium chloride water-alcohol solution, at normal temperatures and pressures, is added in the ammonia saturated alcohol solution that contains ammonium chloride, and reaction generates the magnesium chloride hex-ammoniate precipitation.Because there are shortcomings such as operational path is long, the ammonia consumption is big, productive rate is low in above method, therefore, development of new, the magnesium chloride hex-ammoniate synthetic method has great importance efficiently.
Summary of the invention
The objective of the invention is for a kind of synthesizing magnesium chloride hexammoniate is provided.This method is utilized magnesium silicide and the chemical reaction of anhydrous ammonium chloride in the liquefied ammonia medium, has obtained well-crystallized's magnesium chloride hex-ammoniate, and technology is simple.
The concrete steps of the technical solution used in the present invention are as follows:
1) is after 1: 2～1: 3 the mixed, to put into closed reaction vessel with magnesium silicide and anhydrous ammonium chloride, stirs by mass ratio;
2) feeding quality in above-mentioned reactor is the liquefied ammonia of 2～50 times of magnesium silicide quality, and magnesium silicide and anhydrous ammonium chloride begin to react in the liquefied ammonia medium, and the reaction times is 10 minutes～24 hours;
3) with the gas emptying in the closed reactor, promptly obtained the magnesium chloride hex-ammoniate solid product, chemical formula is MgCl
26NH
3
The beneficial effect that the present invention has is:
Currently used synthesizing magnesium chloride hexammoniate, problem such as have that operational path is long, the ammonia consumption is big and productive rate is low.The present invention utilizes magnesium silicide and the chemical reaction of ammonium chloride in the liquefied ammonia medium, when generating silane gas, has obtained a large amount of magnesium chloride hex-ammoniate by products, and its chemical formula is MgCl
26NH
3, the product well-crystallized.Therefore, the cost that utilizes this method to produce magnesium chloride hex-ammoniate can reduce greatly than additive method, and helps recycling economy.
Description of drawings
Accompanying drawing is the XRD figure spectrum of embodiment 1 gained magnesium chloride hex-ammoniate.
Embodiment
Embodiment 1:
With 10 gram magnesium silicides and 26 gram anhydrous ammonium chloride powder mixes, put into airtight reactor.After reactor vacuumized, feeding quality was the liquefied ammonia of 200 grams, reacts 10 hours.After reaction was finished, with the gas emptying in the reactor, the solid product of acquisition was a magnesium chloride hex-ammoniate, and chemical formula is MgCl
26NH
3Accompanying drawing is the XRD figure spectrum of gained solid product, marks the spacing of all XRD diffraction peak correspondences in the collection of illustrative plates, and (patent No.: the 6143270) data consistent of Gong Buing illustrates that present embodiment gained solid product is a magnesium chloride hex-ammoniate for these data and United States Patent (USP).Simultaneously, the XRD diffraction peak is sharp-pointed, and the product well-crystallized is described.
Embodiment 2:
With 10 gram magnesium silicides and 20 gram anhydrous ammonium chloride powder mixes, put into airtight reactor.After reactor vacuumized, feeding quality was the liquefied ammonia of 500 grams, reacts 10 minutes.After reaction was finished, with the gas emptying in the reactor, the solid product of acquisition was a magnesium chloride hex-ammoniate, and chemical formula is MgCl
26NH
3
Embodiment 3:
With 10 gram magnesium silicides and 30 gram anhydrous ammonium chloride powder mixes, put into airtight reactor.After reactor vacuumized, feeding quality was the liquefied ammonia of 20 grams, reacts 24 hours.After reaction was finished, with the gas emptying in the reactor, the solid product of acquisition was a magnesium chloride hex-ammoniate, and chemical formula is MgCl
26NH
3
Claims (1)
1, a kind of synthesizing magnesium chloride hexammoniate is characterized in that the step of this method is as follows:
1) is after 1: 2～1: 3 the mixed, to put into closed reaction vessel with magnesium silicide and anhydrous ammonium chloride, stirs by mass ratio;
2) feeding quality in above-mentioned reactor is the liquefied ammonia of 2～50 times of magnesium silicide quality, and magnesium silicide and anhydrous ammonium chloride begin to react in the liquefied ammonia medium, and the reaction times is 10 minutes～24 hours;
3) with the gas emptying in the closed reactor, promptly obtained the magnesium chloride hex-ammoniate solid product, chemical formula is MgCl
26NH
3
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100624230A CN101298336A (en) | 2008-06-06 | 2008-06-06 | Synthetic method of magnesium chloride hexammoniate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100624230A CN101298336A (en) | 2008-06-06 | 2008-06-06 | Synthetic method of magnesium chloride hexammoniate |
Publications (1)
| Publication Number | Publication Date |
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| CN101298336A true CN101298336A (en) | 2008-11-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNA2008100624230A Pending CN101298336A (en) | 2008-06-06 | 2008-06-06 | Synthetic method of magnesium chloride hexammoniate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030332B (en) * | 2009-09-30 | 2012-11-21 | 鲍坚仁 | Application of byproducts in preparation of silane through magnesium silicide process |
| CN104724711A (en) * | 2015-02-02 | 2015-06-24 | 上海万寅安全环保科技有限公司 | Manufacturing method for silane type product |
-
2008
- 2008-06-06 CN CNA2008100624230A patent/CN101298336A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030332B (en) * | 2009-09-30 | 2012-11-21 | 鲍坚仁 | Application of byproducts in preparation of silane through magnesium silicide process |
| CN104724711A (en) * | 2015-02-02 | 2015-06-24 | 上海万寅安全环保科技有限公司 | Manufacturing method for silane type product |
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Open date: 20081105 |