CN106477602A - A kind of preparation technology of high-purity low oxychloride magnesium - Google Patents
A kind of preparation technology of high-purity low oxychloride magnesium Download PDFInfo
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- CN106477602A CN106477602A CN201610893032.8A CN201610893032A CN106477602A CN 106477602 A CN106477602 A CN 106477602A CN 201610893032 A CN201610893032 A CN 201610893032A CN 106477602 A CN106477602 A CN 106477602A
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- magnesium
- ammonia
- oxychloride
- purity
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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
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
- C01F5/08—Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide
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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
Abstract
A kind of preparation technology of high-purity low oxychloride magnesium, including step:(1)Using condensation water dissolution magnesium chloride, prepared magnesium chloride solution;(2)Reacted using ammonium chloride and calcium oxide and ammonia after ammonia still process, is obtained;(3)Ammonia is passed through magnesium chloride solution reaction magnesium hydroxide slurry is obtained;(4)Wash magnesium hydroxide slurry using deionized water multistage, after filtration, make filter cake;(5)Using flash distillation dryer, magnesium hydroxide filtration cakes torrefaction is become high purity magnesium hydroxide dry powder;(6)Ammonia still calcium chloride solution out concentrates through filtering post-heating, then makes calcium chloride granules through granulating and drying;(7)Finally high-purity low oxychloride magnesium is obtained using roller kilns calciner.Dangerous materials liquefied ammonia is replaced to do intermediate, the ammonia that ammonium chloride is obtained with lime reaction using ammonium chloride in method provided by the present invention, ammonia and bischofite react high-purity magnesium oxide.Make magnesium oxide product high purity more than 99%, chlorine root, below 0.05%, effectively make use of salt lake resources.
Description
Technical field:
The present invention relates to a kind of process preparing high-purity magnesium oxide, the high-purity magnesium oxide of more particularly, to a kind of low chloride content
Preparation method.
Background technology:
Magnesium oxide is to be a kind of white solid under a kind of ionic compound, room temperature, and high-purity magnesium oxide has excellent at high temperature
Alkali resistance and electrical insulating property, thermal coefficient of expansion and high thermal conductivity, there is good photopermeability.It is widely used in high-temperature flame-proof
Material, is all widely used in the fields such as optics, instrument, electronics, electrical equipment, metallurgy, Aero-Space.
In prior art, the preparation method of high-purity magnesium oxide mainly has:(1)The magnesium mineral resources enriched using northeast, are forged
Burn till common magnesium oxide, then hydrolyze prepared magnesium hydroxide, then filter, wash, pyrolysis obtains high-purity magnesium oxide.In the method by
It is difficult to separate in magnesium hydroxide slurry and washs, lead to impurity content in product higher.(2)By first preparing magnesium chloride or sulfur
Sour magnesium reheating solution prepares magnesium oxide, the high temperature corrosion gas producing in the method, higher to equipment requirements.(3)By carbon ammonium
Circulation method, prepares basic magnesium carbonate, and calcining further produces high-purity magnesium oxide, and the method purity is higher but high cost.(4)Halogen
Water-Method of Soda, magnesium chloride and soda are reacted, and precipitate, through rinsing, centrifuge dehydration, through calcining, pulverizing, selecting crude drugs with winnower, is obtained
Light magnesium oxide, the method chloride content is higher, and side product chlorinated sodium added value is low.(5)Using high-purity magnesium metal and oxygen
Reaction is obtained high-purity micropowder magnesium oxide, and the method is higher to equipment requirements, high cost, and a large amount of production of inapplicable industry.
In the development process of salt lake, predominantly stay in the single potassium chloride utilization of resources, in development process, concentrate discharge
The old halogen containing magnesium cause the Local enrichment of magnesium chloride, have become as to a certain extent exploit resources of salt lakes using during
" magnesium evil ", hampers the exploitation further of salt lake resources.
Content of the invention:
In view of this, the invention provides one kind is with bischofite as raw material, prepare magnesium hydroxide intermediate, then be sintered into high-purity
The method of low oxychloride magnesium, the magnesium chloride that the method is separated out with salt lake bittern, as raw material, produces high purity magnesium hydroxide by ammonia process,
Finally calcining obtains high-purity low oxychloride magnesium, and magnesium oxide purity reaches more than 99%, and chlorine root is below 0.05%.Realize magnesium oxide per ton
Consume 6.7 tons of bischofite raw material, reach making full use of of raw material.
For achieving the above object, the present invention employs the following technical solutions:A kind of preparation work of high-purity low oxychloride magnesium
Skill is it is characterised in that include step:
(1)Using condensation water dissolution magnesium chloride, prepared magnesium chloride solution;
(2)Reacted using ammonium chloride and calcium oxide ammonia still process and ammonia is obtained;
(3)Ammonia is passed through magnesium chloride solution reaction magnesium hydroxide slurry is obtained;
(4)Wash magnesium hydroxide slurry using salt-free water multistage, and make filter cake;
(5)Using flash distillation dryer, magnesium hydroxide filtration cakes torrefaction is become high purity magnesium hydroxide dry powder;
(6)Ammonia still calcium chloride solution out concentrates through filtering post-heating, and then granulating and drying makes calcium chloride granules;
(7)Finally high-purity low oxychloride magnesium is obtained using roller kilns calciner.
The preparation technology of described a kind of high-purity low oxychloride magnesium is it is characterised in that described step(1)In, according to quality
Ratio according to bischofite quality and condensate quality, adjusts solution concentration scope 28-32 ° B é, ensures solution temperature ranges simultaneously
18-22℃.
The preparation technology of described a kind of high-purity low oxychloride magnesium is it is characterised in that described step(2)In, prepare highly concentrated
Degree calcium oxide emulsion, concentration range 120-170tt is reacted with ammonium chloride, steams ammonia in ammonia still, obtains ammonia after cooling,
And it is passed through reactive tank.
The preparation technology of described a kind of high-purity low oxychloride magnesium is it is characterised in that described step(3)In, continuous way is anti-
Answer and in groove, be continuously passed through magnesium chloride solution and ammonia, keep stablizing of reaction, reactive tank stability contorting, at 72-80 DEG C, controls hydrogen
Granularity 50-70 μm of magnesium oxide, particle size span 1.2-1.6.
The preparation technology of described a kind of high-purity low oxychloride magnesium is it is characterised in that described step(4)In, using belt
Filter, multistage counter current is washed, the chlorine root in reduction filter cake to 0.3-0.37%.
The preparation technology of described a kind of high-purity low oxychloride magnesium is it is characterised in that described step(5)In, magnesium hydroxide
Drying adopt flash distillation dryer, using hot-air by drying materials, moisture≤0.5%, then collecting packing.
The preparation technology of described a kind of high-purity low oxychloride magnesium is it is characterised in that described step(6)In, calcium liquid passes through
Three-level concentrates, and concentration reaches 41-43%, is then sent to fluidized bed for spraying, granulating, is dried with hot-air, then collecting packing, is obtained
Side-product calcium chloride.
The preparation technology of described a kind of high-purity low oxychloride magnesium is it is characterised in that described step(7)In, calciner
For New Roller Kiln equipment, magnesium hydroxide calcining heat in kiln controls at 900-1100 DEG C, and calcination time is 8-12 hour, protects
Card product chlorine root is reduced to less than 0.05%.
The preparation technology of the high-purity low oxychloride magnesium of described any one is it is characterised in that described bischofite is Qinghai
Exploit resources of salt lakes carries enrichment old halogen containing magnesium of discharge after potassium.
A kind of calciner preparing high-purity low oxychloride magnesium is it is characterised in that described calciner is roller kilns side
It is provided with air-introduced machine, sack cleaner, cyclone dust extractor, spin vibration sieve and feed(raw material)inlet, finished product is produced;It is fuel using natural gas,
Firing mode is avoid smoke pollution product, magnesium hydroxide is placed in saggar, using roller rod, saggar is sent in kiln, in kiln
It is divided into preheating section, bringing-up section, high temperature section, cooling section, saggar runs about 10h in kiln it is ensured that reaction is complete;Bringing-up section is main
Conversion zone and heat absorption section, high temperature section ensures temperature control at about 1100 DEG C, reduces the chlorine root in product further, and product goes out
Cross 100 eye mesh screens after kiln and send through wind and lower the temperature and pack, roller adopts recrystallized silicon carbide roller rod, and roller transports, and the outer work of kiln
Sequence connects together, Automated condtrol;Burning and temperature control adopt PID intelligence instrument, can very easily adjust and surely
Determine sintering curve;Equipment adopts light heat insulation material.
Advantages of the present invention and effect are:
The present invention compared with prior art, replaces harmful influence liquefied ammonia to do intermediate using ammonium chloride in the method that the present invention provides,
The ammonia that ammonium chloride is obtained with lime reaction, ammonia and bischofite react high-purity magnesium oxide, and ammonia reuses.Using industry
Change continuous reaction groove, improve the stability of product.Adopt new-type calcining equipments so that magnesium oxide product high purity 99% with
On, chlorine root is below 0.05%, the method process is simple, and cost is relatively low, effectively make use of salt lake resources.
Brief description:
The preparation technology flow chart of a kind of high-purity low oxychloride magnesium that Fig. 1 is provided by the embodiment of the present invention.
Fig. 2 is the structural representation of calciner of the present invention.
Specific embodiment:
Below in conjunction with specific embodiment, the present invention is described in further detail:
Referring to the drawings shown in 1-2, the present invention relates to a kind of preparation technology of high-purity low oxychloride magnesium is it is characterised in that include step
Suddenly:
(1)Using condensation water dissolution magnesium chloride, prepared magnesium chloride solution;
(2)Reacted using ammonium chloride and calcium oxide ammonia still process and ammonia is obtained;
(3)Ammonia is passed through magnesium chloride solution reaction magnesium hydroxide slurry is obtained;
(4)Wash magnesium hydroxide slurry using salt-free water multistage, and make filter cake;
(5)Using flash distillation dryer, magnesium hydroxide filtration cakes torrefaction is become high purity magnesium hydroxide dry powder;
(6)Ammonia still calcium chloride solution out concentrates through filtering post-heating, and then granulating and drying makes calcium chloride granules;
(7)Finally high-purity low oxychloride magnesium is obtained using roller kilns calciner.
The preparation technology of described a kind of high-purity low oxychloride magnesium,
Preferably, step(1)In, adjust magnesium chloride solution concentration range 28-32 ° B é, ensure solution temperature ranges 18-22 simultaneously
DEG C, filtered it is ensured that the purity of magnesium chloride solution using pressure filter and accurate filter.
Preferably, step(2)In, prepare high concentration calcium oxide emulsion concentration scope 120-170tt, react with ammonium chloride,
Steam ammonia in ammonia still, after deionized water condensation, obtain ammonia.
Preferably, step(3)In, reaction container is produced using continuity method it is ensured that the stablizing of reaction condition and magnesium hydroxide, control
Granularity 50-70 μm of hydrogen manufacturing magnesium oxide, span 1.2-1.6.
Preferably, step(4)In, using band filter, multistage counter current is washed, the chlorine root in reduction filter cake to 0.3-
0.37%.
Preferably, step(5)In, the drying of magnesium hydroxide adopts flash distillation dryer, moisture≤0.5% after drying, so
Collecting packing afterwards.
Preferably, step(6)In, calcium liquid concentrates through three-level, and concentration reaches 41-43%, is then sent to fluidized bed for spraying and makes
Grain, is dried with hot-air, then collecting packing, prepared side-product calcium chloride.
Preferably, step(7)In, calciner is New Roller Kiln equipment, and calcining heat is about in kiln for magnesium hydroxide
900-1100 DEG C, calcination time is 8-12 hour, and continuous way produces it is ensured that product is stable, magnesium oxide chlorine root be reduced to 0.05% with
Under.
The preparation technology of the high-purity low oxychloride magnesium of described any is it is characterised in that described bischofite is Qinghai
Exploit resources of salt lakes carries enrichment old halogen containing magnesium of discharge after potassium.
A kind of calciner preparing high-purity low oxychloride magnesium is it is characterised in that described calciner is roller kilns side
It is provided with air-introduced machine, sack cleaner, cyclone dust extractor, spin vibration sieve and feed(raw material)inlet, finished product is produced;It is fuel using natural gas,
Firing mode is avoid smoke pollution product, magnesium hydroxide is placed in saggar, using roller rod, saggar is sent in kiln, in kiln
It is divided into preheating section, bringing-up section, high temperature section, cooling section, saggar runs about 10h in kiln it is ensured that reaction is complete;Bringing-up section is main
Conversion zone and heat absorption section, high temperature section ensures temperature control at about 1100 DEG C, reduces the chlorine root in product further, and product goes out
Cross 100 eye mesh screens after kiln and send through wind and lower the temperature and pack, roller adopts recrystallized silicon carbide roller rod, and roller transports, and the outer work of kiln
Sequence connects together, Automated condtrol;Burning and temperature control adopt PID intelligence instrument, can very easily adjust and surely
Determine sintering curve;Equipment adopts light heat insulation material.
Embodiment 1
1. by magnesium chloride solids condensation water dissolution, according to mass ratio, according to bischofite quality and condensate quality, adjust molten
Liquid concentration range 28-32 ° B é, is passed through 18-22 DEG C of solution temperature ranges of guarantee simultaneously.
2. prepare high concentration calcium oxide emulsion concentration scope 120-170tt to react with ammonium chloride, steam ammonia in ammonia still
Gas, obtains ammonia after condensation, and is passed through reactive tank.
3. continuously it is passed through magnesium chloride solution and ammonia in continuous reaction groove, keep stablizing of reaction, reactive tank is stably controlled
Make at 72-80 DEG C, magnesium hydroxide granularity 50-70 μm, particle size span 1.2-1.6.
4. react the suspension obtaining and deliver to belt vacuum filter, extract liquid out with vacuum pump, and be washed with deionized water
Wash filter cake, reduce magnesium hydroxide chlorine root, filtrate is mainly ammonium chloride solution, deliver to the continuation of chloride leach pond anti-with calcium oxide
Should, recycling.
5. magnesium hydroxide filter cake is delivered in flash distillation dryer and is dried, moisture≤0.5% after drying, and removes through cloth bag
Dirt device and cyclone dust extractor collecting packing.
6. ammonium chloride and calcium oxide react generation calcium chloride and ammonia, and calcium chloride solution after filtering, delivers to concentration section
It is concentrated into concentration about 43%, then uses hot-air granulating and drying in fluid bed, obtain calcium chloride product, packaging, sell, it is to avoid
Pollution environment.
7. magnesium hydroxide dry powder is sent in roller kilns and calcine, roller kilns carry out to traditional roller kilns for my company breakthrough
Improve and the novel device of designed, designed, be fuel using natural gas, firing mode is avoid smoke pollution product, hydrogen-oxygen
Change magnesium to be placed in saggar, sent into saggar in kiln using roller rod, in kiln, be divided into preheating section, bringing-up section, high temperature section, cooling section, casket
Alms bowl runs about 10h in kiln it is ensured that reaction is complete;Bringing-up section is main conversion zone and heat absorption section, and high temperature section ensures temperature
Control at about 1100 DEG C, reduce the chlorine root in product further, cross 100 eye mesh screens after product kiln discharge and send through wind and lower the temperature and wrap
Dress.Roller adopts recrystallized silicon carbide roller rod, has thermal field equilibrium, and surface temperature is low, and gradient of temperature is fast, and energy-conserving and environment-protective etc. are excellent
Point;Roller transport can reduce handling product in kiln, and the outer operation of kiln connects together, easy to operate, have very high automatic simultaneously
Change control level;Burning and temperature control adopt PID intelligence instrument, can very easily adjust and stablize sintering curve;
Equipment adopts light heat insulation material, and heat conductivity is low, greatly reduces kiln body radiating, improves heat utilization ratio, reduce product
The energy consumption of product.
The above, the only present invention preferably specific embodiment, protection scope of the present invention not limited to this, any familiar
Those skilled in the art in the technical scope of present disclosure, the technical scheme that can become apparent to simple
Change or equivalence replacement each fall within protection scope of the present invention.
Claims (10)
1. a kind of preparation technology of high-purity low oxychloride magnesium is it is characterised in that include step:
(1)Using condensation water dissolution magnesium chloride, prepared magnesium chloride solution;
(2)Reacted using ammonium chloride and calcium oxide ammonia still process and ammonia is obtained;
(3)Ammonia is passed through magnesium chloride solution reaction magnesium hydroxide slurry is obtained;
(4)Wash magnesium hydroxide slurry using salt-free water multistage, and make filter cake;
(5)Using flash distillation dryer, magnesium hydroxide filtration cakes torrefaction is become high purity magnesium hydroxide dry powder;
(6)Ammonia still calcium chloride solution out concentrates through filtering post-heating, and then granulating and drying makes calcium chloride granules;
(7)Finally high-purity low oxychloride magnesium is obtained using roller kilns calciner.
2. a kind of preparation technology of high-purity low oxychloride magnesium according to claim 1 is it is characterised in that described step(1)
In, according to mass ratio, according to bischofite quality and condensate quality, adjust solution concentration scope 28-32 ° B é, ensure simultaneously
18-22 DEG C of solution temperature ranges.
3. a kind of preparation technology of high-purity low oxychloride magnesium according to claim 1 is it is characterised in that described step(2)
In, prepare high concentration calcium oxide emulsion, concentration range 120-170tt is reacted with ammonium chloride, steams ammonia in ammonia still, cooling
Obtain ammonia afterwards, and be passed through reactive tank.
4. a kind of preparation technology of high-purity low oxychloride magnesium according to claim 1 is it is characterised in that described step(3)
In, continuously it is passed through magnesium chloride solution and ammonia in continuous reaction groove, keep stablizing of reaction, reactive tank stability contorting is in 72-
80 DEG C, control granularity 50-70 μm of magnesium hydroxide, particle size span 1.2-1.6.
5. a kind of preparation technology of high-purity low oxychloride magnesium according to claim 1 is it is characterised in that described step(4)
In, using band filter, multistage counter current is washed, the chlorine root in reduction filter cake to 0.3-0.37%.
6. a kind of preparation technology of high-purity low oxychloride magnesium according to claim 1 is it is characterised in that described step(5)
In, the drying of magnesium hydroxide adopts flash distillation dryer, using hot-air by drying materials, moisture≤0.5%, then collecting packing.
7. a kind of preparation technology of high-purity low oxychloride magnesium according to claim 1 is it is characterised in that described step(6)
In, calcium liquid concentrates through three-level, and concentration reaches 41-43%, is then sent to fluidized bed for spraying, granulating, is dried with hot-air, Ran Houshou
Collection packaging, prepared side-product calcium chloride.
8. a kind of preparation technology of high-purity low oxychloride magnesium according to claim 1 is it is characterised in that described step(7)
In, calciner is New Roller Kiln equipment, and magnesium hydroxide calcining heat in kiln controls at 900-1100 DEG C, and calcination time is
8-12 hour is it is ensured that product magnesium oxide chlorine root is reduced to less than 0.05%.
9. the preparation technology of the high-purity low oxychloride magnesium of any according to claim 1-8 is it is characterised in that described water
Chloromagnesite carries enrichment old halogen containing magnesium of discharge after potassium for Qinghai Salt Lake development of resources.
10. a kind of calciner preparing high-purity low oxychloride magnesium described in claim 1 is it is characterised in that described calciner
It is that roller kilns side is provided with air-introduced machine, sack cleaner, cyclone dust extractor, spin vibration sieve and feed(raw material)inlet, finished product is produced;Using
Natural gas is fuel, is to avoid smoke pollution product, magnesium hydroxide is placed in saggar on firing mode, using roller rod by saggar
Sending in kiln, being divided into preheating section, bringing-up section, high temperature section, cooling section in kiln, saggar runs about 10h it is ensured that having reacted in kiln
Entirely;Bringing-up section is main conversion zone and heat absorption section, and high temperature section ensures temperature control at about 1100 DEG C, reduces product further
In chlorine root, cross 100 eye mesh screens after product kiln discharge and send through wind and lower the temperature and pack, roller adopts recrystallized silicon carbide roller rod, roller
Son transport, and outside kiln, operation connects together, Automated condtrol;Burning and temperature control adopt PID intelligence instrument, can be very
Easily adjust and stablize sintering curve;Equipment adopts light heat insulation material.
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Cited By (3)
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CN106986359A (en) * | 2017-05-22 | 2017-07-28 | 河北镁神科技有限公司 | The device and method of chlorinity in product magnesia is reduced in a kind of magnesium hydroxide calcination process |
CN108190924A (en) * | 2018-02-11 | 2018-06-22 | 中南大学 | A kind of preparation method for reducing magnesium hydroxide chlorinity |
CN115771908A (en) * | 2022-11-23 | 2023-03-10 | 北京化工大学 | Preparation method of low-chlorine magnesium hydroxide |
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CN106986359A (en) * | 2017-05-22 | 2017-07-28 | 河北镁神科技有限公司 | The device and method of chlorinity in product magnesia is reduced in a kind of magnesium hydroxide calcination process |
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