CN110002480A - A kind of method of anhydrous production poly-aluminum chloride-magnesium - Google Patents
A kind of method of anhydrous production poly-aluminum chloride-magnesium Download PDFInfo
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- CN110002480A CN110002480A CN201910245866.1A CN201910245866A CN110002480A CN 110002480 A CN110002480 A CN 110002480A CN 201910245866 A CN201910245866 A CN 201910245866A CN 110002480 A CN110002480 A CN 110002480A
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- magnesium
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- chloride
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- aluminum chloride
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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
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- 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
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to environmental protection treatment agent technical fields, more particularly to a kind of method of anhydrous production poly-aluminum chloride-magnesium.With quick, small, the small advantage of exhaust gas of pollution.A kind of method of anhydrous production poly-aluminum chloride-magnesium, the following steps are included: step 1: using magnesium-containing mineral/mineral or other magnesium materials that contain as step, 350 DEG C to 900 DEG C at a temperature of be selectively plasticized, plastication obtains magnesium chloride mixing and squeezes out solvent ammonium chloride, reaction mixture 90% is dissolved in polar organic solvent, 10% or 10% or less is suspended, and polar organic solvent is anhydrous state solvent;Step 2: selectively anhydrous state solvent being leaked out magnesium and be blended in squeeze out in solvent at it from analysis in above-mentioned plastification material and isolates insoluble impurity, the two is separated;Step 3: passing through NATE dehydrated precipitate chlorination magnesate;Step 4: being handled in a crystallizer as excess ammonia;Step 5: the suspension filtering that step 4 obtains squeezes out Isolating chlorinated magnesium in solvent using centrifugal process in centrifuge.
Description
Technical field
The present invention relates to environmental protection treatment agent technical fields, more particularly to a kind of method of anhydrous production poly-aluminum chloride-magnesium.
Background technique
The production of existing safety door can generally remain two kinds of objects, one is the aluminium skin residue of exterior skin, and it is internal every
Sound and insulation filling materials, aluminium skin residue can be used to recycle, and include again magnesium alloy in aluminium skin, have when production
Particulate matter and magnesium alloy powder generate, and the recycling of these waste products can also generate economic benefit.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of method of anhydrous production poly-aluminum chloride-magnesium,
With quick, small, the small advantage of exhaust gas of pollution.
The method of the anhydrous production poly-aluminum chloride-magnesium of one kind proposed by the present invention, comprising the following steps:
Step 1: using magnesium-containing mineral/mineral or it is other containing magnesium material as step, 350 DEG C to 900 DEG C at a temperature of selectively mould
To change, plastication obtains magnesium chloride mixing and squeezes out solvent ammonium chloride, reaction mixture 90% is dissolved in polar organic solvent,
10% or 10% or less is suspended, and polar organic solvent is anhydrous state solvent;
Step 2: selectively anhydrous state solvent is analysed from above-mentioned plastification material leak out magnesium and its be blended in squeeze out it is molten
Insoluble impurity is isolated in agent, and the two is separated;
Step 3: passing through NATE dehydrated precipitate chlorination magnesate;
Step 4: and handled in a crystallizer as excess ammonia;
Step 5: the suspension that step 4 obtains is filtered, and is being utilized between 25000 turns ~ 17000 turns in centrifuge using centrifugation
Method squeezes out Isolating chlorinated magnesium in solvent and obtains magnesium chloride fluid mixture;
Step 6: heating isolate thermal decomposition chlorination magnesate in evaporator and magnesium chloride and ammonium hydroxide is precipitated, dehydration takes off ammonium hydroxide
Out, the anhydrous magnesium chloride below of water content 0.1% is obtained.
203.30 category 1.56 ~ 1.59g/m3 of density monoclinic system of step 7 detection, MgCl2.6H2O: >=98%;MgCl2:≥
46%;Sulfate :≤0.6%;Alkali metal chloride :≤1.2%;Calcium :≤0.14%;Water-insoluble: being completely dissolved in water, in second
In alcohol: being completely dissolved;
Step 8, detection packaging shipment.
It is that methanol or methanol and calcium chloride are suspension mixed one or more as the preferred polar organic solvent.
Contain amount that is identical as in stoichiometry or being more than as extrusion solvent needed for the preferred optional leakage grade
The amount of the mg and NH 4cl of dissolution.
Squeezing out solvent as the ammonium hydroxide isolated in the preferred magnesium chloride fluid mixture can repeat in the method
Recycling uses, and the method for being dehydrated and being handled before the solvent being collected into is reused.
Squeezing out solvent as preferably optional ammonium hydroxide is conversion in dissolution polar organic solvent (anhydrous condition) to be added chlorine is precipitated
Change ammonium.
As preferably due to ammonium chloride with from pyrolysis step collect ammonia and hydrochloric acid reactant salt, come carry out recycling and it is harmless
Processing.
It is dissolved as 4 ammonium chloride of preferred steps in polar organic solvent (anhydrous condition), and the electrolytic salt from chlorine
Acid.
C as all replenishers needed for excessive ammonia treatment substantive operations needed for preferred steps 4lThe method of introducing
For Cl2、HClAnd NH4The acid anhydrides of Cl or MgCl2 form or hydrate.
It is additionally added replenishers in step 4 as the preferred ammonium chloride, replenishers use NH3(g) or 4 c of NHl's
It is one or more.
Compared with prior art, the present invention has the beneficial effects that the finished product transparency after dry is high, richness
Good, hardness is adjustable, admittedly in the water-free system contained, keeping higher purity, the material used is harmless as far as possible, can solve pollution
Lead to the problem of, solve may the presence of aqueous treatment be precipitated that difficulty demand repeats or consumptive material consumption is excessive, generation
A series of problems, such as product yellowing is heterochromatic.
Specific embodiment
Below by embodiment, preferred specific description is used as to technical solution of the present invention:
Embodiment 1:
The method of the anhydrous production poly-aluminum chloride-magnesium of one kind proposed by the present invention, comprising the following steps:
Step 1: using magnesium-containing mineral/mineral or it is other containing magnesium material as step, 350 DEG C to 900 DEG C at a temperature of selectively mould
To change, plastication obtains magnesium chloride mixing and squeezes out solvent ammonium chloride, reaction mixture 90% is dissolved in polar organic solvent,
10% or 10% or less is suspended, and polar organic solvent is anhydrous state solvent;
Step 2: selectively anhydrous state solvent is analysed from above-mentioned plastification material leak out magnesium and its be blended in squeeze out it is molten
Insoluble impurity is isolated in agent, and the two is separated;
Step 3: passing through NATE dehydrated precipitate chlorination magnesate;
Step 4: and handled in a crystallizer as excess ammonia;
Step 5: the suspension that step 4 obtains is filtered, and is being utilized between 25000 turns ~ 17000 turns in centrifuge using centrifugation
Method squeezes out Isolating chlorinated magnesium in solvent and obtains magnesium chloride fluid mixture;
Step 6: heating isolate thermal decomposition chlorination magnesate in evaporator and magnesium chloride and ammonium hydroxide is precipitated, dehydration takes off ammonium hydroxide
Out, the anhydrous magnesium chloride below of water content 0.1% is obtained.
203.30 category 1.56 ~ 1.59g/m3 of density monoclinic system of step 7 detection, MgCl2.6H2O: >=98%;MgCl2:≥
46%;Sulfate :≤0.6%;Alkali metal chloride :≤1.2%;Calcium :≤0.14%;Water-insoluble: being completely dissolved in water, in second
In alcohol: being completely dissolved;
Step 8, detection packaging shipment.
Embodiment 2
A kind of method of anhydrous production poly-aluminum chloride-magnesium, comprising the following steps:
Step 1: using magnesium-containing mineral/mineral or it is other containing magnesium material as step, 350 DEG C to 900 DEG C at a temperature of selectively mould
To change, plastication obtains magnesium chloride mixing and squeezes out solvent ammonium chloride, reaction mixture 90% is dissolved in polar organic solvent,
10% or 10% or less is suspended, and polar organic solvent is suspension mixed for methanol and calcium chloride, and is anhydrous state solvent;
Step 2: selectively anhydrous state solvent is analysed from above-mentioned plastification material leak out magnesium and its be blended in squeeze out it is molten
Insoluble impurity is isolated in agent, and the two is separated;
Step 3: passing through NATE dehydrated precipitate chlorination magnesate;
Step 4: and handled in a crystallizer as excess ammonia;
Step 5: the suspension that step 4 obtains is filtered, and is being utilized between 25000 turns ~ 17000 turns in centrifuge using centrifugation
Method squeezes out Isolating chlorinated magnesium in solvent and obtains magnesium chloride fluid mixture;The ammonium hydroxide isolated in magnesium chloride fluid mixture squeezes out
Solvent can repeat recycling in the method and use, and the method for being dehydrated and being handled before the solvent being collected into is reused;
Step 6: heating isolate thermal decomposition chlorination magnesate in evaporator and magnesium chloride and ammonium hydroxide is precipitated, dehydration takes off ammonium hydroxide
Out, the anhydrous magnesium chloride below of water content 0.1% is obtained.
203.30 category 1.56 ~ 1.59g/m3 of density monoclinic system of step 7 detection, MgCl2.6H2O: >=98%;MgCl2:≥
46%;Sulfate :≤0.6%;Alkali metal chloride :≤1.2%;Calcium :≤0.14%;Water-insoluble: being completely dissolved in water, in second
In alcohol: being completely dissolved;
Step 8, detection packaging shipment.
Embodiment 3
A kind of method of anhydrous production poly-aluminum chloride-magnesium, comprising the following steps:
Step 1: using magnesium-containing mineral/mineral or it is other containing magnesium material as step, 350 DEG C to 900 DEG C at a temperature of selectively mould
To change, plastication obtains magnesium chloride mixing and squeezes out solvent ammonium chloride, reaction mixture 90% is dissolved in polar organic solvent,
10% or 10% or less is suspended, and polar organic solvent is suspension mixed for methanol and calcium chloride, and is anhydrous state solvent;
Step 2: selectively anhydrous state solvent is analysed from above-mentioned plastification material leak out magnesium and its be blended in squeeze out it is molten
Insoluble impurity is isolated in agent, and the two is separated;
Step 3: passing through NATE dehydrated precipitate chlorination magnesate;Dehydration squeezes out solvent and contains identical as in stoichiometry or be more than
Amount dissolution mg and NH 4cl amount;
Step 4: and handled in a crystallizer as excess ammonia;
Step 5: the suspension that step 4 obtains is filtered, and is being utilized between 25000 turns ~ 17000 turns in centrifuge using centrifugation
Method squeezes out Isolating chlorinated magnesium in solvent and obtains magnesium chloride fluid mixture;The ammonium hydroxide isolated in magnesium chloride fluid mixture squeezes out
Solvent can repeat recycling in the method and use, and the method for being dehydrated and being handled before the solvent being collected into is reused;
It is conversion in dissolution polar organic solvent (anhydrous condition) to be added ammonium chloride is precipitated that ammonium hydroxide, which squeezes out solvent,;Ammonium chloride is walked with from pyrolysis
Suddenly the ammonia and hydrochloric acid reactant salt collected have no harm reason to carry out recycling;
Step 6: heating isolate thermal decomposition chlorination magnesate in evaporator and magnesium chloride and ammonium hydroxide is precipitated, dehydration takes off ammonium hydroxide
Out, the anhydrous magnesium chloride below of water content 0.1% is obtained.
203.30 category 1.56 ~ 1.59g/m3 of density monoclinic system of step 7 detection, MgCl2.6H2O: >=98%;MgCl2:≥
46%;Sulfate :≤0.6%;Alkali metal chloride :≤1.2%;Calcium :≤0.14%;Water-insoluble: being completely dissolved in water, in second
In alcohol: being completely dissolved;
Step 8, detection packaging shipment.
Embodiment 4, a kind of method of anhydrous production poly-aluminum chloride-magnesium, comprising the following steps:
Step 1: using magnesium-containing mineral/mineral or it is other containing magnesium material as step, 350 DEG C to 900 DEG C at a temperature of selectively mould
Change, plastication obtains magnesium chloride mixing and squeezes out solvent ammonium chloride, and ammonium chloride is carried out at polar organic solvent (anhydrous condition)
Dissolution, and reaction mixture 90% is dissolved in polar organic solvent from hydrochloric acid is electrolysed in chlorine, 10% or 10% or less suspended, pole
Property organic solvent be anhydrous state solvent;
Step 2: selectively anhydrous state solvent is analysed from above-mentioned plastification material leak out magnesium and its be blended in squeeze out it is molten
Insoluble impurity is isolated in agent, and the two is separated;
Step 3: passing through NATE dehydrated precipitate chlorination magnesate;
Step 4: and handled in a crystallizer as excess ammonia;All replenishers needed for excessive ammonia treatment substantive operations
ClThe method of introducing is Cl2、HClAnd NH4The acid anhydrides of Cl or MgCl2 form or hydrate;Replenishers have been additionally added, have been supplemented
Agent uses NH3(g) or 4 c of NHlIt is one or more;
Step 5: the suspension that step 4 obtains is filtered, and is being utilized between 25000 turns ~ 17000 turns in centrifuge using centrifugation
Method squeezes out Isolating chlorinated magnesium in solvent and obtains magnesium chloride fluid mixture;
Step 6: heating isolate thermal decomposition chlorination magnesate in evaporator and magnesium chloride and ammonium hydroxide is precipitated, dehydration takes off ammonium hydroxide
Out, the anhydrous magnesium chloride below of water content 0.1% is obtained.
203.30 category 1.56 ~ 1.59g/m3 of density monoclinic system of step 7 detection, MgCl2.6H2O: >=98%;MgCl2:≥
46%;Sulfate :≤0.6%;Alkali metal chloride :≤1.2%;Calcium :≤0.14%;Water-insoluble: being completely dissolved in water, in second
In alcohol: being completely dissolved;
Step 8, detection packaging shipment.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (10)
1. a kind of method of anhydrous production poly-aluminum chloride-magnesium, it is characterized in that: the following steps are included:
Step 1: using magnesium-containing mineral/mineral or it is other containing magnesium material as step, 350 DEG C to 900 DEG C at a temperature of selectively mould
To change, plastication obtains magnesium chloride mixing and squeezes out solvent ammonium chloride, reaction mixture 90% is dissolved in polar organic solvent,
10% or 10% or less is suspended, and polar organic solvent is anhydrous state solvent;
Step 2: selectively anhydrous state solvent is analysed from above-mentioned plastification material leak out magnesium and its be blended in squeeze out it is molten
Insoluble impurity is isolated in agent, and the two is separated;
Step 3: passing through NATE dehydrated precipitate chlorination magnesate;
Step 4: and handled in a crystallizer as excess chlorination ammonia;
Step 5: the suspension that step 4 obtains is filtered, and is being utilized between 25000 turns ~ 17000 turns in centrifuge using centrifugation
Method squeezes out Isolating chlorinated magnesium in solvent and obtains magnesium chloride fluid mixture;
Step 6: heating isolate thermal decomposition chlorination magnesate in evaporator and magnesium chloride and ammonium hydroxide is precipitated, dehydration takes off ammonium hydroxide
Out, the anhydrous magnesium chloride below of water content 0.1% is obtained.
2. 203.30 category 1.56 ~ 1.59g/m3 of density monoclinic system of step 7 detection, MgCl2.6H2O: >=98%;MgCl2:≥
46%;Sulfate :≤0.6%;Alkali metal chloride :≤1.2%;Calcium :≤0.14%;Water-insoluble: being completely dissolved in water, in second
In alcohol: being completely dissolved;
Step 8, detection packaging shipment.
3. the method for the anhydrous production poly-aluminum chloride-magnesium of one kind according to claim 1, it is characterized in that: the polarity is organic molten
Agent is that methanol or methanol and calcium chloride are suspension mixed one or more.
4. the method for the anhydrous production poly-aluminum chloride-magnesium of one kind according to claim 1, it is characterized in that: the extrusion solvent contains
There is the amount of the mg and NH 4cl of the dissolution of amount that is identical as in stoichiometry or being more than.
5. the method for the anhydrous production poly-aluminum chloride-magnesium of one kind according to claim 1, it is characterized in that: the magnesium chloride fluid
The ammonium hydroxide isolated in mixture squeezes out solvent can repeat recycling use in the method, be taken off before the solvent being collected into
Water and the method for processing are reused.
6. a kind of method of anhydrous production poly-aluminum chloride-magnesium according to claim 1 or 5, it is characterized in that: optional ammonium hydroxide squeezes
Solvent is conversion in dissolution polar organic solvent (anhydrous condition) to be added ammonium chloride is precipitated out.
7. the method for the anhydrous production poly-aluminum chloride-magnesium of one kind according to claim 6, it is characterized in that: due to ammonium chloride with from
The ammonia and hydrochloric acid reactant salt that pyrolysis step is collected have no harm reason to carry out recycling.
8. the method for the anhydrous production poly-aluminum chloride-magnesium of one kind according to claim 1, it is characterized in that: step 4 ammonium chloride exists
Polar organic solvent (anhydrous condition) is dissolved, and hydrochloric acid is electrolysed from sal-ammoniac.
9. the method for the anhydrous production poly-aluminum chloride-magnesium of one kind according to claim 1, it is characterized in that: the mistake needed for step 4
The C of all replenishers needed for measuring chlorination ammonia treatment substantive operationslThe method of introducing is Cl2、HClAnd NH4Cl or MgCl2
The acid anhydrides of form or hydrate.
10. the method for the anhydrous production poly-aluminum chloride-magnesium of one kind according to claim 1, it is characterized in that: the ammonium chloride exists
Replenishers are additionally added in step 4, replenishers use NH3(g) or 4 c of NHlIt is one or more.
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Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1229400A (en) * | 1997-06-20 | 1999-09-22 | 挪威海德罗公开有限公司 | Process for producing anhydrous MgC12 |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN1229400A (en) * | 1997-06-20 | 1999-09-22 | 挪威海德罗公开有限公司 | Process for producing anhydrous MgC12 |
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