CN107500319A - A kind of preparation method of anhydrous magnesium chloride - Google Patents
A kind of preparation method of anhydrous magnesium chloride Download PDFInfo
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- CN107500319A CN107500319A CN201710819107.2A CN201710819107A CN107500319A CN 107500319 A CN107500319 A CN 107500319A CN 201710819107 A CN201710819107 A CN 201710819107A CN 107500319 A CN107500319 A CN 107500319A
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- magnesium chloride
- anhydrous 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
- C01F5/26—Magnesium halides
- C01F5/30—Chlorides
- C01F5/34—Dehydrating magnesium chloride containing water of crystallisation
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Abstract
The invention discloses a kind of preparation method of anhydrous magnesium chloride, it includes step：S1, bischofite is mixed to acquisition dehydrated raw material with ammonium chloride；S2, dehydrated raw material carried out at 180 DEG C~240 DEG C successively to carry out second dehydration at primary dewatering and 250 DEG C~300 DEG C, obtain anhydrous magnesium chloride crude product；S3, after white cigarette around anhydrous magnesium chloride crude product disappears, anhydrous magnesium chloride crude product is warming up under protective atmosphere not less than 250 DEG C and is incubated at least 2h, obtain anhydrous magnesium chloride；Wherein, in step S2, S3, there is no gas overflowing reaction system.Preparation in accordance with the present invention, using ammonium chloride as protective agent, the ammonia and hydrogen chloride gas that are thermally decomposed into using it, hydrogen chloride gas can suppress hydrolysis, the hydrone in the replaceable hydrated magnesium chloride of ammonia, be relatively beneficial to the acquisition of anhydrous magnesium chloride.The preparation method is simple and easy, cost is cheap, and avoids the problem of equipment corrosion under the conditions of the high-temperature closed caused by simple hydrogen chloride gas method is serious.
Description
Technical field
The invention belongs to salt lake resources technical field of comprehensive utilization, it relates in particular to a kind of preparation of anhydrous magnesium chloride
Method.
Background technology
Magnesium and magnesium alloy have many excellent processing and performance, and production Technology and application study are increasingly drawn
Play the concern of people.Application in fields such as space flight and aviation, automobile, electronics, communication instrument is increasing, is described as " 21 century
Green engineering structural metallic materials ".At present, anhydrous magnesium chloride electrolytic preparation magnesium metal is the optimised process of metal Magnesium Industry
Route, but wherein anhydrous magnesium chloride raw material prepares difficult, production cost height, causes the magnesium or magnesium alloy cost height produced,
Product lacks the market competitiveness.
Production electrolysis anhydrous magnesium chloride mainly has following several method at present：
(1) hydrogen chloride gas Protection Code：This method is using hydrogen chloride as protective gas, by dewatering bischofite into anhydrous chlorine
Change magnesium, the effect of hydrogen chloride is to suppress the generation of magnesium chloride dihydrate hydrolysis generation basic magnesium chloride；Hydrogen chloride protective atmosphere
It is considered as production method optimal at present that lower dehydration, which prepares anhydrous magnesium chloride, and its dewatering process product quality is very high, and environment is dirty
Contaminate relatively small, production process is easily controlled, and still, hydrogen chloride, vapor and other corrosivity gas can be discharged in dehydration
The tail gas such as body, in order to reduce cost and avoid environmental pollution, hydrogen chloride is recycled in production process；At present using condensation parsing
Method removing tail gas in moisture, this technique is high to equipment requirement, complex operation, and investment cost is big.
(2) magnesia chlorinated with chlorine method：This method be use carry potassium after old halogen for raw material, it is dry by removal of impurities concentration, spraying
The methods of dry, prepares magnesium chloride dihydrate, and the chlorination in chlorinator after a certain amount of carbon, two water chlorine will be added in magnesium chloride dihydrate
Changing the magnesia that magnesium generates in dehydration can occur to react as follows with chlorine：
2MgO+C+2Cl2(g)→2MgCl2+CO2(g)
(3) chlorination hydrogen chloride molten magnesium chloride method：This method is leached the magnesium in serpentine using hydrochloric acid, obtains magnesium chloride
Solution, through cleaning, concentrating, the process such as mist projection granulating obtain magnesium chloride dihydrate；Magnesium chloride dihydrate is passed through in chlorination furnace molten again
Melt and hydrogen chlorination is chlorinated under state；The magnesia of production generates anhydrous magnesium chloride, chlorine in chlorinator with hcl reaction
Change gas harvest watery hydrochloric acid out in device；Reaction equation is as follows：
MgCl2·2H2O→MgCl2+2H2O(g)
MgCl2·2H2O→MgO+2HCl(g)+H2O(g)
MgO+2HCl(g)→MgCl2+H2O(g)
(4) the ammonia process dehydration of bischofite：MgCl2Can be corresponding to many organic solvents such as alcohol, ether, amine, fat effect generation
Complex compound (such as with methanol generate MgCl2·6CH3OH, MgCl is generated with ethanol2·6C2H5OH), and act on and generating with ammonia
MgCl2·6NH3、MgCl2·4NH3、MgCl2·2NH3Deng complex compound；During heating, these complex compounds can decompose again, so as to
It can obtain anhydrous magnesium chloride；The technique uses the small ammonia of corrosivity to avoid very scabrous hydrogen chloride pair for dehydration mediators
The etching problem of equipment, but organic solvent is introduced, environment certainly will be polluted.
At the same time, salt lake resources have abundant bischofite resource；Salt lake is exploited always based on sylvite in decades,
The substantially no comprehensive exploitation of other salt lake mineral products or exploitation have the gesture of gradual atrophy, if magnesium resource is for a long time because of techno-economic question
Industrialized production can not be put into, only Cha Er Han Salt Lake has nearly 5,000,000,000 tons of chlorination magnesium resource, the 1 ton of chlorination of production every year of lake region enterprise
Potassium, it will attach and produce 10 tons of magnesium chlorides.
Therefore, the recycling problem of the bischofite based on a large amount of by-products in Salt Lake Area and above-mentioned existing by six water chlorine
Change magnesium and prepare the technique drawback of anhydrous magnesium chloride, finding a kind of can simply be prepared into anhydrous magnesium chloride by bischofite is cheap
Technique, it is urgent problem to be solved.
The content of the invention
, should the invention provides a kind of preparation method of anhydrous magnesium chloride to solve the above-mentioned problems of the prior art
Preparation method using bischofite as raw material, and after being decomposed by ammonium chloride product and inert atmosphere protective effect, not only make
Bischofite is obtained in dehydration from hydrolysis, is more easy to obtain the higher anhydrous magnesium chloride of purity.
In order to reach foregoing invention purpose, present invention employs following technical scheme：
A kind of preparation method of anhydrous magnesium chloride, it is characterised in that including step：
S1, bischofite is mixed to acquisition dehydrated raw material with ammonium chloride；
S2, the dehydrated raw material is carried out to primary dewatering at 180 DEG C~240 DEG C, obtain magnesium chloride dihydrate crude product；
S3, the magnesium chloride dihydrate crude product is carried out to second dehydration at 250 DEG C~300 DEG C, it is thick to obtain anhydrous magnesium chloride
Product；
S4, after around the anhydrous magnesium chloride crude product white cigarette disappear after, by the anhydrous magnesium chloride crude product in protective atmosphere
Under be incubated at least 2h at not less than 250 DEG C, obtain anhydrous magnesium chloride；
Wherein, in the step S2~S4, there is no gas overflowing reaction system.
Further, in the dehydrated raw material, the mass ratio of the bischofite and the ammonium chloride is 1:1~1:5.
Further, in the step S4, the protective atmosphere is any one in argon gas, nitrogen, helium.
Further, the step S2~S4 is carried out in closed container.
Further, the step S2~S4 is carried out in condensation reflux unit.
The present invention controls acid extraction by the solid mixture by heating bischofite and ammonium chloride, its
Middle ammonium chloride is thermally decomposed into ammonia and hydrogen chloride gas, and hydrogen chloride gas can effectively suppress the hydrolysis of magnesium chloride, is promoted
Enter the progress of bischofite dehydration generation anhydrous magnesium chloride；The preparation method using substep directly heats, it is simple and easy, into
This is cheap, can efficiently prepare anhydrous magnesium chloride, for prepare electrolysis produce metal magnesium industry provide practical, cheap raw material without
Aqueous magnesium chloride；And decompose obtained ammonia and can regenerate chloride solid after hydrogen chloride gas cooling, easily recovery；With showing
There is hydrogen chloride gas Protection Code in technology to compare, under the reaction condition for avoiding high-temperature closed, hydrogen chloride gas heavy corrosion is set
The problem of standby；Meanwhile preparation method of the invention not only reduces the wasting of resources with giving up using salt lake by-product bischofite as raw material
Thing pollutes, and the added value that salt lake resources utilize also greatly improved.In addition, process similar in compared with prior art,
Preparation in accordance with the present invention uses gas-solid reaction, and the method for adding ammonium chloride produces protective atmosphere hydrogen chloride, by direct
The mode of heating makes bischofite Direct Dehydration, while employs inert gas shielding, simple to operate, and products obtained therefrom purity is high.
Embodiment
Hereinafter, embodiments of the invention are described in detail in the future.However, it is possible to implement this hair in many different forms
It is bright, and the specific embodiment of the invention that should not be construed as limited to illustrate here.Conversely, there is provided these embodiments be for
The principle and its practical application of the present invention is explained, so that others skilled in the art are it will be appreciated that the present invention's is various
Embodiment and the various modifications for being suitable for specific intended application.
It will be appreciated that although term " once ", " secondary " etc. can be used to describe various technological operations herein, still
These technological operations should not be limited by these terms.These terms are only used for a technological operation and another identical work
Skill operation makes a distinction.
Embodiment 1
First, bischofite is mixed with ammonium chloride and obtains dehydrated raw material, wherein, the dosage of bischofite and ammonium chloride is
It is 1 according to the corresponding mass of anhydrous magnesium chloride in bischofite and the mass ratio of ammonium chloride:2.
Then, above-mentioned dehydrated raw material is warming up to 180 DEG C, insulation reaction 1h with 1 DEG C/min heating rate, carried out once
Dehydration, obtain magnesium chloride dihydrate crude product.
During primary dewatering, bischofite sloughs outermost two free waters first, generates four aqueous magnesium chlorides；So
Slough the hydrone of two medium adhesions of centre again afterwards, generate magnesium chloride dihydrate.And in the process, heated point of ammonium chloride
Solution can suppress the hydrolysis of magnesium chloride dihydrate into ammonia and hydrogen chloride gas, hydrogen chloride gas.
Again, magnesium chloride dihydrate crude product is continuously heating to 250 DEG C, insulation reaction 3h, carries out second dehydration, obtained anhydrous
Magnesium chloride crude product.
During magnesium chloride dihydrate thermal dehydration, it may occur that partial hydrolysis, the reaction such as following formula occurs：
MgCl2·2H2O→MgOHCl+HCl(g)+H2O(g)
The hydrogen chloride gas that ammonium chloride is obtained by thermal decomposition can effectively suppress above-mentioned hydrolytic process, so as to ensure that acquisition
The purity of anhydrous magnesium chloride crude product.
Finally, white cigarette disappearance is heated to, argon gas is passed through and 2h is incubated at 250 DEG C, sealed up for safekeeping after cooling, obtain anhydrous chlorination
Magnesium.
It is relatively low to meet temperature during upward overflow for the ammonia and hydrogen chloride gas that ammonium chloride is obtained by thermal decomposition
Reactor wall and regenerate ammonium chloride, produce white cigarette, after white cigarette disappearance, that is, complete ammonium chloride laid equal stress on by thermal decomposition it is new cold
The process of solidifying generation ammonium chloride；Meanwhile during above-mentioned second dehydration, can typically there are the bad feelings that can not be dehydrated completely
Condition, therefore, after the protective effect of hydrogen chloride gas is terminated, by the way of protective atmosphere is passed through, make the water not being dehydrated completely
Close magnesium chloride and be further dehydrated generation anhydrous magnesium chloride, so as to further improve product purity.
What deserves to be explained is when carrying out above-mentioned dehydration in the present embodiment, using open heating, can preferably use cold
Solidifying reflux, to prevent ammonia that ammonium chloride thermally decomposed to generate and hydrogen chloride gas from overflowing reaction system.
Products obtained therefrom is analyzed, wherein water insoluble matter content (wt%) is 5.82%；Also, products obtained therefrom is through XRD
Analysis understands that product principal component is anhydrous magnesium chloride.
Embodiment 2
It in the description of embodiment 2, will not be repeated here, only described with embodiment 1 not with the something in common of embodiment 1
Same part.The difference of embodiment 2 and embodiment 1 is that first, the dosage of bischofite and ammonium chloride is according to water chlorine magnesium
The corresponding mass of anhydrous magnesium chloride and the mass ratio of ammonium chloride are 1 in stone:3；Secondly, the temperature of primary dewatering is 200 DEG C, and
Insulation reaction 3h, obtain magnesium chloride dihydrate crude product；Again, the temperature of second dehydration is 300 DEG C, and insulation reaction 2h；Finally, treat
White cigarette is passed through argon gas after disappearing and 3h is incubated at 250 DEG C, seals acquisition anhydrous magnesium chloride after cooling up for safekeeping.
Products obtained therefrom is analyzed, wherein water insoluble matter content (wt%) is 2.06%；Also, product through XRD
Analysis understands that product principal component is anhydrous magnesium chloride.
Embodiment 3
It in the description of embodiment 3, will not be repeated here, only described with embodiment 1 not with the something in common of embodiment 1
Same part.The difference of embodiment 3 and embodiment 1 is that first, the dosage of bischofite and ammonium chloride is according to water chlorine magnesium
The corresponding mass of anhydrous magnesium chloride and the mass ratio of ammonium chloride are 1 in stone:4；Secondly, the temperature of primary dewatering is 220 DEG C, and
Insulation reaction 4h, obtain magnesium chloride dihydrate crude product；Again, the temperature of second dehydration is 280 DEG C, and insulation reaction 2h；Finally, treat
White cigarette is passed through argon gas after disappearing and 2h is incubated at 250 DEG C, seals acquisition anhydrous magnesium chloride after cooling up for safekeeping.
Products obtained therefrom is analyzed, wherein water insoluble matter content (wt%) is 1.00%；Also, product through XRD
Analysis understands that product principal component is anhydrous magnesium chloride.
Embodiment 4
It in the description of embodiment 4, will not be repeated here, only described with embodiment 1 not with the something in common of embodiment 1
Same part.The difference of embodiment 4 and embodiment 1 is that first, the dosage of bischofite and ammonium chloride is according to water chlorine magnesium
The corresponding mass of anhydrous magnesium chloride and the mass ratio of ammonium chloride are 1 in stone:5；Secondly, the temperature of primary dewatering is 240 DEG C, and
Insulation reaction 1h, obtain magnesium chloride dihydrate crude product；Again, the temperature of second dehydration is 260 DEG C, and insulation reaction 3h；Finally, treat
White cigarette is passed through argon gas after disappearing and 3h is incubated at 250 DEG C, seals acquisition anhydrous magnesium chloride after cooling up for safekeeping.
Products obtained therefrom is analyzed, wherein water insoluble matter content (wt%) is 0.94%；Also, product through XRD
Analysis understands that product principal component is anhydrous magnesium chloride.
Embodiment 5
It in the description of embodiment 5, will not be repeated here, only described with embodiment 1 not with the something in common of embodiment 1
Same part.The difference of embodiment 5 and embodiment 1 is that first, the dosage of bischofite and ammonium chloride is according to water chlorine magnesium
The corresponding mass of anhydrous magnesium chloride and the mass ratio of ammonium chloride are 1 in stone:4；Secondly, the temperature of primary dewatering is 190 DEG C, and
Insulation reaction 3h, obtain magnesium chloride dihydrate crude product；Again, the temperature of second dehydration is 260 DEG C, and insulation reaction 2h；Finally, treat
White cigarette is passed through argon gas after disappearing and 2h is incubated at 250 DEG C, seals acquisition anhydrous magnesium chloride after cooling up for safekeeping.
Products obtained therefrom is analyzed, wherein water insoluble matter content (wt%) is 0.92%；Also, product through XRD
Analysis understands that product principal component is anhydrous magnesium chloride.
What deserves to be explained is although the preparation process of anhydrous magnesium chloride employs condensing reflux in above-described embodiment 1-5
The open mode of heating of device, but can also be entered according to the preparation method of the anhydrous magnesium chloride of the present invention in closed container
OK, so to prevent ammonia that ammonium chloride thermally decomposed to generate and hydrogen chloride gas from overflowing reaction system.
Although the present invention has shown and described with reference to specific embodiment, it should be appreciated by those skilled in the art that：
In the case where not departing from the spirit and scope of the present invention limited by claim and its equivalent, can carry out herein form and
Various change in details.
Claims (5)
1. a kind of preparation method of anhydrous magnesium chloride, it is characterised in that including step：
S1, bischofite is mixed to acquisition dehydrated raw material with ammonium chloride；
S2, the dehydrated raw material is carried out to primary dewatering at 180 DEG C~240 DEG C, obtain magnesium chloride dihydrate crude product；
S3, the magnesium chloride dihydrate crude product is carried out to second dehydration at 250 DEG C~300 DEG C, obtain anhydrous magnesium chloride crude product；
S4, after around the anhydrous magnesium chloride crude product white cigarette disappear after, by the anhydrous magnesium chloride crude product under protective atmosphere in
At least 2h is incubated at not less than 250 DEG C, obtains anhydrous magnesium chloride；
Wherein, in the step S2~S4, there is no gas overflowing reaction system.
2. preparation method according to claim 1, it is characterised in that in the dehydrated raw material, in the bischofite
The mass ratio of magnesium chloride and the ammonium chloride is 1:1~1:5.
3. preparation method according to claim 1, it is characterised in that in the step S4, the protective atmosphere is argon
Any one in gas, nitrogen, helium.
4. according to any described preparation methods of claim 1-3, it is characterised in that the step S2~S4 is in closed container
Carry out.
5. according to any described preparation methods of claim 1-3, it is characterised in that the step S2~S4 fills in condensing reflux
Put middle progress.
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| CN201710819107.2A CN107500319A (en) | 2017-09-12 | 2017-09-12 | A kind of preparation method of anhydrous magnesium chloride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109607581A (en) * | 2019-02-19 | 2019-04-12 | 河北工业大学 | A kind of device and method for producing anhydrous magnesium chloride using ammonium chloride and magnesium carbonate |
| CN113214801A (en) * | 2021-05-19 | 2021-08-06 | 中国科学院上海应用物理研究所 | Low cost MgCl based on bischofite2Preparation method of (E) -KCl eutectic salt |
| CN113479917A (en) * | 2021-08-02 | 2021-10-08 | 青海盐湖工业股份有限公司 | Method and system for preparing anhydrous magnesium chloride |
| CN113479916A (en) * | 2021-08-02 | 2021-10-08 | 青海盐湖工业股份有限公司 | Method and system for large-scale production of anhydrous magnesium chloride |
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|---|---|---|---|---|
| CN101555028A (en) * | 2009-05-11 | 2009-10-14 | 湖南理工学院 | Method for preparing high purity anhydrous magnesium chloride by gas-solid reaction |
| CN104418370A (en) * | 2013-09-03 | 2015-03-18 | 中国科学院过程工程研究所 | Method and device for preparing anhydrous magnesium chloride |
| CN106673029A (en) * | 2017-03-07 | 2017-05-17 | 辽宁工程技术大学 | Method for producing high-purity anhydrous magnesium chloride by using bischofite |
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2017
- 2017-09-12 CN CN201710819107.2A patent/CN107500319A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555028A (en) * | 2009-05-11 | 2009-10-14 | 湖南理工学院 | Method for preparing high purity anhydrous magnesium chloride by gas-solid reaction |
| CN104418370A (en) * | 2013-09-03 | 2015-03-18 | 中国科学院过程工程研究所 | Method and device for preparing anhydrous magnesium chloride |
| CN106673029A (en) * | 2017-03-07 | 2017-05-17 | 辽宁工程技术大学 | Method for producing high-purity anhydrous magnesium chloride by using bischofite |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109607581A (en) * | 2019-02-19 | 2019-04-12 | 河北工业大学 | A kind of device and method for producing anhydrous magnesium chloride using ammonium chloride and magnesium carbonate |
| CN109607581B (en) * | 2019-02-19 | 2023-08-29 | 河北工业大学 | Device and method for preparing anhydrous magnesium chloride by using ammonium chloride and magnesium carbonate |
| CN113214801A (en) * | 2021-05-19 | 2021-08-06 | 中国科学院上海应用物理研究所 | Low cost MgCl based on bischofite2Preparation method of (E) -KCl eutectic salt |
| CN113479917A (en) * | 2021-08-02 | 2021-10-08 | 青海盐湖工业股份有限公司 | Method and system for preparing anhydrous magnesium chloride |
| CN113479916A (en) * | 2021-08-02 | 2021-10-08 | 青海盐湖工业股份有限公司 | Method and system for large-scale production of anhydrous magnesium chloride |
| CN113479916B (en) * | 2021-08-02 | 2022-09-16 | 青海盐湖工业股份有限公司 | Method and system for large-scale production of anhydrous magnesium chloride |
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Application publication date: 20171222 |