CN104556156B - 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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Abstract
A kind of preparation method of anhydrous magnesium chloride, it is preliminary first under HCl gas shields that low hydrate is obtained by the dehydration of magnesium chloride hyperhydrate, residual water is removed by chemical reaction then high-purity anhydrous magnesium chloride is obtained.Preliminary hydro-extraction temperature is relatively low, it is ensured that magnesium chloride does not occur to greatly reduce energy consumption while hydrolysis；In chemical reaction dehydration, dehydrant is obtained by sulfur, chlorine reaction, and intermediate species is constantly recycled, and chemical reaction dehydration makes product anhydrous magnesium chloride thoroughly depart from water environment, the side reaction product SO of generation2, HCl be gas, fundamentally avoid the generation of hydrolysis.This raw materials technology wide material sources are cheap, and whole technological process is good in economic efficiency, there is provided method strong operability, be easily achieved industrialization.
Description
Technical field
The present invention relates to a kind of preparation method of magnesium compound, more particularly to a kind of preparation method of anhydrous magnesium chloride.
Background technology
Magnesium is one of most light structural metallic material, with specific strength and specific stiffness it is high, damping and amortization and machinability are good, be easy to
The advantages of recovery, it is widely used in automobile making, electronic product, aerospace industry and military field etc..Electrolysis prepares magnesium metal
Current development technique faster, its primary raw material are anhydrous magnesium chloride.It is magnesium chloride hyperhydrate wide material sources, cheap, lead to
It will be a kind of desirable feedstock to cross dehydration and anhydrous magnesium chloride is obtained.By taking magnesium chloride hexahydrate as an example, which prepares the dehydration of anhydrous magnesium chloride
Process is as follows：
MgCl2·6H2O=MgCl2·4H2O+2H2O↑
MgCl2·4H2O=MgCl2·2H2O+2H2O↑
MgCl2·2H2O=MgCl2·H2O+H2O↑
MgCl2·H2O=MgCl2+H2O↑
Wherein easily there are hydrolysis in the lower hydrate of magnesium chloride hexahydrate in dehydration：
MgCl2·H2O=Mg (OH) Cl+HCl ↑
Mg (OH) Cl=MgO+HCl ↑
The Thermal Decomposition Mechanism being dehydrated from magnesium chloride hexahydrate, MgC12·6H2O takes off to low water and is easier to, in hot-air
Can just achieve the goal；But Magnesium chloride with low water dehydration is more difficult, during dehydration, part can occur hydrolysis.As hydrolysis are generated
Magnesium oxide, product cannot meet the production requirement of electrolysis refining magnesium.In how suppressing dehydration, hydrolysis are to carry
The key of high anhydrous magnesium chloride purity.
Magnesium chloride hexahydrate dehydration at present prepares the process study of anhydrous magnesium chloride mainly includes following direction：
Protection thermal dehydration method, i.e., be dehydrated under chlorine or hydrogen chloride gas protection.Patent CN1234608C,
This kind of method that CN102275960B is mainly adopted.At a certain temperature, maintain the dense of chlorine or hydrogen chloride in heating systems
Degree is minimum so as to hydrolysis during high temperature are reduced to.Under HCl protective atmospheres dewatering process due to environmental pollution it is little, produced
Process control high degree of automation, therefore for relatively advanced dewatering.Dehydration under protective gas can be a certain degree of
Suppress the generation of hydrolysis, but in the industrial production, this kind of technique has certain limitation, needs in dehydration
Very high temperature, energy consumption are larger, and equipment seriously corroded under high temperature, and part HC1 gases and water recovery are in MgC12Product
On, affect product quality.
Double salt method, the reaction such as hydrated magnesium chloride and potassium chloride, ammonium chloride is first made the Carnallite KCl of double salt structure
MgC12·6H2O, ammonium carnallite NH4CI·MgC12·6H2O.Patent CN1326773C, CN1156398C, CN102491384B,
CN 102491383B mainly adopt the method.As the activity of magnesium chloride in carnallite is significantly than magnesium chloride in hydrated magnesium chloride
It is active little, in dehydration, hydrolysis are significantly reduced, so as to improve the quality of anhydrous magnesium chloride.The dehydration of carnallite point
Step is carried out, and with the rising of temperature, the water in carnallite constantly loses, and last anhydrous magnesium chloride.Due to double salt structure
Effect, in making every step dehydration, equilibrium vapor partial pressure is easier to dehydration much larger than the equilibrium vapor partial pressure value of magnesium chloride hexahydrate
Carry out and hydrolysis do not occur.This method partial oxidation when ammonium chloride is reclaimed decomposes or hydrolyzes the corrosive hydrogen chloride of generation,
NH4The trapping of CI dust, free NH3Recovery, improve NH4The aspects such as the CI response rate also have that a large amount of needs are perfect.
Method of substitution, i.e., first use ammonia, alcohol equimolecular to replace MgC12·6H2Hydrone in O, forms MgC12·6NH3, then
Replacement molecule is removed again so as to anhydrous magnesium chloride is obtained.Patent CN1043215C, CN101462746B mainly adopts the method.The method
In order to eliminating water needs to heat the alcoholic solution of magnesium chloride, ammonia, alcoholic solution all can only partly replace water, and replace completely needs hydrone
Need substantial amounts of alcohol, this not only consumes substantial amounts of energy, while solution can produce wax-like aggregation in heating process, make magnesium chloride and
Alcohol cannot be kept completely separate, it can be seen that said method realizes that industrialization has many difficulties.
Not enough for the shortcoming of prior art, this patent proposes to prepare high-pure anhydrous chlorine using magnesium chloride hexahydrate using one kind
The technique for changing magnesium.
The content of the invention
Present invention solves the technical problem that be overcome prior art in prepare anhydrous chlorination with the high hydrate of magnesium chloride
During magnesium, the difficult facile hydrolysiss of intermediate product Magnesium chloride with low water dehydration, to be difficult to improve end-product purity, power consumption, high cost, equipment easy
The shortcomings of being corroded, there is provided a kind of with low cost, process is simple and effective generation for suppressing hydrolysis in dehydration, raising
The preparation method of anhydrous magnesium chloride purity.
To solve above-mentioned technical problem, the present invention adopts following technical proposals：
A kind of preparation method of anhydrous magnesium chloride, including physics intensification dehydration and chemical reaction two stages of dehydration, it is described
Physics intensification dehydration be the slow intensification magnesium chloride hyperhydrate under hci gas flow protection, preliminary removing part water generating
Magnesium chloride lower hydrate MgC12·xH2The process of O；The chemical reaction dehydration refers to the MgC1 of generation2·xH2O is in thionyl
The process of anhydrous magnesium chloride is generated in the presence of chlorine.
Its specific step of preparation process includes：
1), under HCl air-flow protections, slow intensification magnesium chloride hyperhydrate, preliminary removing part water generating magnesium chloride are low
Hydrate MgC12·xH2O；
2), by Cl2With the S from follow-up rectification section2Cl2Mixing, makes S2Cl2It is converted into SCl2；
3), by step 2) obtained by SCl2In adding the reactor of jacketed, the SO returned with follow-up workshop section2It is synthesized
SOCl2；
4), the product that 3) rectification step obtains, after rectification, bottom of towe is SOCl2, tower top is unreacted SCl2；
5), by step 4) SOCl2 that obtains is passed into step 1) obtained by low hydrate MgC12xH2O in, occur
Chemical reaction dehydration obtains the high-pure anhydrous MgCl2 of product.
The advantage of the preparation technology is embodied in the byproduct of reaction of each step of preparation technology and can reclaim or recycle, specifically
It is embodied in：
1), step of preparation process 1) in dehydration after carry secretly steam HCl Jing absorb become byproduct hydrochloric acid；
2), step of preparation process 4) in unreacted SCl2S is obtained by S beds2Cl2, return to step of preparation process 2)
Middle participation conversion and cycle；
3), step of preparation process 5) in generate SO2Gas returns to step 3) in conversion and cycle, the HCl gases of generation
Return to step 1) in as physics heat up dehydration protective gas.
The major parameter of each step of the preparation technology is：
Physics heats up and is dehydrated in the lower hydrate MgC12xH2O for obtaining, and the numerical range of x is 0.5<x<2.5, dehydration temperature
Spend for 100～300 DEG C；S2Cl2It is converted into SCl2Temperature be 55～75 DEG C；SO2SOCl is synthesized2Temperature be 150～250
DEG C, it is that thermal cycle oil is passed through in the reactor of described jacketed that temperature maintains method；SOCl2Rectification temperature be 50～
150℃；SOCl2With MgC12·xH2The reaction temperature of O is 60～100 DEG C.
Above-mentioned technical proposal is adopted, the beneficial effects of the present invention is：
Magnesium chloride hyperhydrate is prepared high-purity anhydrous magnesium chloride and is dehydrated using two steps, and preliminary hydro-extraction is protected in hci gas flow
Lower removing part water, dehydration temperaturre are lower than traditional snead process about 200 DEG C, big while ensureing that magnesium chloride does not occur hydrolysis
Reduce greatly energy consumption；Final dewatering is dehydrated for chemical reaction, reacts the SO for generating2, HCl be gas, make product anhydrous magnesium chloride
Thoroughly depart from water environment, fundamentally avoid the generation of hydrolysis, while the gas for generating is easy to and anhydrous chlorination
Magnesium products are separated；This raw materials technology wide material sources are cheap, and can consume the serious superfluous chlorine of chlorine industry and converted
For byproduct hydrochloric acid, in technological process, sulfur is recycled with different shape, and whole technological process is good in economic efficiency, there is provided method
Strong operability, it is easily achieved industrialization.
Description of the drawings
Fig. 1 is the process chart of method for preparation of anhydrous magnesium chloride provided in an embodiment of the present invention.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with accompanying drawing and it is embodied as
Example, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is used only for explaining this
It is bright, it is not intended to limit the present invention.
Fig. 1 is referred to, Fig. 1 is the process chart of the preparation method of anhydrous magnesium chloride provided in an embodiment of the present invention, from
Visible in Fig. 1, the preparation method of anhydrous magnesium chloride comprises the steps：
1) magnesium chloride hyperhydrate is carried out into physics intensification dehydration, obtains magnesium chloride lower hydrate MgC12·xH2O；
Specifically, under HCl air-flow protections, magnesium chloride hyperhydrate is slowly heated up in fluid bed, tentatively removing portion
Divide the low hydrate MgC1 of water generating2·xH2O；
Preferably, magnesium chloride hyperhydrate is MgC12·6H2O, it can be understood as the present invention magnesium chloride hyperhydrate be
MgC12·6H2O；
Wherein, in the lower hydrate MgC12xH2O for obtaining, the numerical range of x is 0.5<x<2.5；
Wherein, the temperature of physics intensification dehydration is 100～300 DEG C；
Wherein, the HCl Jing absorptions for carrying steam after dehydration secretly become byproduct hydrochloric acid.
2) by Cl2With S2Cl2Mixing, makes S2Cl2Conversion obtains SCl2；
Specifically, Cl is passed through under conditions of 55～75 DEG C2With the S from follow-up rectification section2Cl2Mixing, is allowed to react
By S2Cl2Change into SCl2。
3) by SCl2With SO2Mixing, reaction generate SOCl2；
Specifically, under conditions of 150～250 DEG C, make step 2) obtained by SCl2The SO returned with follow-up workshop section2Reaction
Synthesis SOCl2；
Wherein, SCl2With SO2Mixing generates SOCl2Reaction be to carry out in the reactor of jacketed；
Wherein, SCl2With SO2Mixing generates SOCl2Reaction temperature to maintain method be reactor in described jacketed
In be passed through thermal cycle oil.
4) rectification SOCl2,It is allowed to and unreacted SCl2Separate；
Specifically, under conditions of 50～150 DEG C, by step 3) product that obtains is passed through rectifying column and carries out rectification,
Bottom of towe obtains SOCl2, top gaseous phase light component is mainly SCl2；
Wherein, tower top light component obtains S by S beds2Cl2, return to step 2) and middle participation conversion and cycle；
5)SOCl2With low hydrate MgC12·xH2O reactions obtain high-pure anhydrous MgCl2；
Specifically, under conditions of 60～100 DEG C, by step 4) SOCl that obtains2Be passed into step 1) obtained by low water
Compound Mg C12·xH2In O, there is chemical reaction dehydration and obtain the high-pure anhydrous MgCl of product2；
Wherein, byproduct of reaction SO2Gas returns to step 3) in conversion and cycle；
Wherein, byproduct of reaction HCl gases return to step 1) in as magnesium chloride hyperhydrate physics heat up dehydration
Protective gas.
Embodiment 1：
Under HCl air-flow protections, magnesium chloride hyperhydrate is to slowly warm up to into 100 DEG C in fluid bed, tentatively removing portion
Divide the low hydrate MgC1 of water generating2·xH2O；Cl is passed through under conditions of 55 DEG C2With the S from follow-up rectification section2Cl2It is mixed
Close, be allowed to react S2Cl2Change into SCl2；Under conditions of 150 DEG C, the SCl that above-mentioned reaction is obtained2Return with follow-up workshop section
The SO for returning2SOCl is synthesized2；Under conditions of 50 DEG C, the product that above-mentioned steps are obtained is passed through rectifying column carries out essence
Evaporate, bottom of towe obtains SOCl2；Under conditions of 60 DEG C, by the SOCl for obtaining2It is passed through the low hydrate that physics biologically dehydrating is obtained
MgC12·xH2In O, there is chemical reaction dehydration and obtain the high-pure anhydrous MgCl of product2。
Embodiment 2：
Under HCl air-flow protections, magnesium chloride hyperhydrate is to slowly warm up to into 200 DEG C in fluid bed, tentatively removing portion
Divide the low hydrate MgC1 of water generating2·xH2O；Cl is passed through under conditions of 65 DEG C2With the S from follow-up rectification section2Cl2It is mixed
Close, be allowed to react S2Cl2Change into SCl2；Under conditions of 200 DEG C, the SCl that above-mentioned reaction is obtained2Return with follow-up workshop section
The SO for returning2SOCl is synthesized2；Under conditions of 100 DEG C, the product that above-mentioned steps are obtained is passed through rectifying column carries out essence
Evaporate, bottom of towe obtains SOCl2；Under conditions of 80 DEG C, by the SOCl for obtaining2It is passed through the low hydrate that physics biologically dehydrating is obtained
MgC12·xH2In O, there is chemical reaction dehydration and obtain the high-pure anhydrous MgCl of product2。
Embodiment 3：
Under HCl air-flow protections, magnesium chloride hyperhydrate is to slowly warm up to into 300 DEG C in fluid bed, tentatively removing portion
Divide the low hydrate MgC1 of water generating2·xH2O；Cl is passed through under conditions of 75 DEG C2With the S from follow-up rectification section2Cl2It is mixed
Close, be allowed to react S2Cl2Change into SCl2；Under conditions of 250 DEG C, the SCl that above-mentioned reaction is obtained2Return with follow-up workshop section
The SO for returning2SOCl is synthesized2；Under conditions of 150 DEG C, the product that above-mentioned steps are obtained is passed through rectifying column carries out essence
Evaporate, bottom of towe obtains SOCl2；Under conditions of 100 DEG C, by the SOCl for obtaining2It is passed through the low hydrate that physics biologically dehydrating is obtained
MgC12·xH2In O, there is chemical reaction dehydration and obtain the high-pure anhydrous MgCl of product2。
Embodiment 4：
Under HCl air-flow protections, by MgC12·6H2O is to slowly warm up to 150 DEG C in fluid bed and is kept for 10 minutes, continues
It is warming up to 250 DEG C to be kept for 20 minutes, dehydration generates low hydrate MgC12·2H2O；By Cl2With from follow-up rectification section
S2Cl2Mixing, it is 60 DEG C to control temperature, S2Cl2It is converted into SCl2；The SCl of gained2It is in adding the reactor of jacketed, and follow-up
The SO that workshop section returns2SOCl is synthesized2, it is passed through thermal cycle oil to derive the heat that reaction is generated in reacting kettle jacketing, remains anti-
Temperature is answered to be 200 DEG C；By the SOCl for obtaining2With unreacted SCl2Rectification separation is carried out, rectification temperature is obtained for 80 DEG C of bottom of towe
SOCl2, top gaseous phase light component is mainly SCl2；The SOCl for obtaining2It is passed into the low hydrate that physics heats up obtained by dehydration
MgC12·2H2In O, there is chemical reaction under the conditions of 80 DEG C, be dehydrated obtain product purity be 99.6% it is anhydrous
MgCl2。
Embodiment 5：
Under HCl air-flow protections, by MgC12·6H2O is to slowly warm up to 180 DEG C in fluid bed and is kept for 20 minutes, continues
It is warming up to 250 DEG C to be kept for 30 minutes, dehydration generates low hydrate MgC12·H2O；By Cl2With from follow-up rectification section
S2Cl2Mixing, it is 70 DEG C to control temperature, S2Cl2It is converted into SCl2；The SCl of gained2It is in adding the reactor of jacketed, and follow-up
The SO that workshop section returns2SOCl is synthesized2, it is passed through thermal cycle oil to derive the heat that reaction is generated in reacting kettle jacketing, remains anti-
Temperature is answered to be 180 DEG C；By the SOCl for obtaining2With unreacted SCl2Rectification separation is carried out, rectification temperature is 70 DEG C, and bottom of towe is obtained
SOCl2, top gaseous phase light component is mainly SCl2；By the SOCl for obtaining2It is passed into the low hydrate that physics intensification dehydration is obtained
MgC12·H2In O, there is chemical reaction under the conditions of 100 DEG C, be dehydrated obtain product purity be 99.8% it is anhydrous
MgCl2。
The above, is only presently preferred embodiments of the present invention, not makees any pro forma restriction to invention, although this
It is bright disclosed above with preferred embodiment, but the present invention is not intended to limit, any those skilled in the art, not
Depart from the range of technical solution of the present invention, become when a little change being made using the technology contents of the disclosure above or being modified to equivalent
The Equivalent embodiments of change, as long as being, without departing from technical solution of the present invention content, to implement to more than according to the technical spirit of the present invention
Any simple modification, equivalent variations and modification that example is made, still fall within the range of technical solution of the present invention.
Claims (8)
1. a kind of preparation method of anhydrous magnesium chloride, including physics heats up dehydration and chemical reaction two stages of dehydration, its feature
It is：Described physics intensification dehydration is slow intensification magnesium chloride hyperhydrate, tentatively removing portion under hci gas flow protection
Divide water generating magnesium chloride lower hydrate MgC12·xH2The process of O；The chemical reaction dehydration refers to the MgC1 of generation2·xH2O
The process of anhydrous magnesium chloride is generated in the presence of thionyl chloride；The preparation method of the anhydrous magnesium chloride includes preparing work as follows
Skill：
1), under HCl air-flow protections, slow intensification magnesium chloride hyperhydrate is preliminary to remove the low hydration of part water generating magnesium chloride
Thing MgC12·xH2O；
2), by Cl2With the S from follow-up rectification section2Cl2Mixing, makes S2Cl2It is converted into SCl2；
3), by step 2) obtained by SCl2In adding the reactor of jacketed, the SO returned with follow-up workshop section2It is synthesized
SOCl2；
4), the product that 3) rectification step obtains, after rectification, bottom of towe is SOCl2, tower top is unreacted SCl2；
5), by step 4) SOCl that obtains2Be passed into step 1) obtained by low hydrate MgC12·xH2In O, there is chemistry anti-
Should be dehydrated and obtain the high-pure anhydrous MgCl of product2。
2. the preparation method of a kind of anhydrous magnesium chloride according to claim 1, it is characterised in that each step of preparation technology
Byproduct of reaction can be reclaimed or be recycled, including：
1), step of preparation process 1) in dehydration after carry secretly steam HCl Jing absorb become byproduct hydrochloric acid；
2), step of preparation process 4) in unreacted SCl2S is obtained by S beds2Cl2, ginseng in returning to step of preparation process 2)
With conversion and cycle；
3), step of preparation process 5) in generate SO2Gas returns to step 3) in conversion and cycle, the HCl gases of generation return to
Step 1) in as physics heat up dehydration protective gas.
3. a kind of preparation method of anhydrous magnesium chloride according to claim 1, it is characterised in that lower hydrate MgC12·
xH2In O, the numerical range of x is 0.5<x<2.5.
4. the preparation method of a kind of anhydrous magnesium chloride according to claim 1, it is characterised in that physics heats up the temperature of dehydration
Spend for 100～300 DEG C.
5. a kind of preparation method of anhydrous magnesium chloride according to claim 1, it is characterised in that S2Cl2It is converted into SCl2's
Temperature is 55～75 DEG C.
6. a kind of preparation method of anhydrous magnesium chloride according to claim 1, it is characterised in that SO2SOCl is synthesized2
Temperature be 150～250 DEG C, temperature maintain method be passed through in the reactor of described jacketed thermal cycle oil.
7. a kind of preparation method of anhydrous magnesium chloride according to claim 1, it is characterised in that SOCl2Rectification temperature be
50～150 DEG C.
8. a kind of preparation method of anhydrous magnesium chloride according to claim 1, it is characterised in that SOCl2With MgC12·
xH2The reaction temperature of O is 60～100 DEG C.
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