CN108502906A - A kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide - Google Patents
A kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide Download PDFInfo
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- CN108502906A CN108502906A CN201810562030.XA CN201810562030A CN108502906A CN 108502906 A CN108502906 A CN 108502906A CN 201810562030 A CN201810562030 A CN 201810562030A CN 108502906 A CN108502906 A CN 108502906A
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- acid
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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
- C01F5/14—Magnesium hydroxide
- C01F5/20—Magnesium hydroxide by precipitation from solutions of magnesium salts with ammonia
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide, is related to a kind of method preparing magnesium hydroxide, using light burnt powder as raw material, with certain density waste acid liquor（Hydrochloric acid, nitric acid, sulfuric acid etc.）Mixing carries out the molten reaction of acid in certain condition, certain density magnesium salt solution is made, magnesium salts refined liquid is obtained using removal of impurities, is allowed to react with the ammonia being passed through in the bubbling style reactor with stirring, control ammonia flow, stir speed (S.S.) and reaction temperature.After a certain period of time, reaction solution is aged through constant temperature, obtains magnesium hydrate powder after filtration washing and drying process for reaction.Ammonia in filtrate can prepare the ammonia used during magnesium sinking by crystallization reaction, to realize the cycle of ammonia；Ammonium salt in filtrate can prepare ammonium salt product by crystallization reaction.This technique products obtained therefrom is high-quality, and operating procedure is simple, and equipment is taken up an area less, and production cost is low, and pollutant discharge amount is small, is suitable for large-scale production, is a kind of technology in prepared by high purity magnesium hydroxide.
Description
Technical field
The present invention relates to a kind of methods preparing magnesium hydroxide, and high-purity hydrogen-oxygen is prepared more particularly to a kind of molten light burnt powder of acid
Change the method for magnesium.
Background technology
Magnesium hydroxide is a kind of highly important inorganic compound, and environment friendly and pollution-free, development potentiality is huge, using extensive,
Consumption increases year by year, has higher economic value and social value.Wherein, the application field of high purity magnesium hydroxide is increasingly
Extensively, it is to produce various high purity magnesium hydroxide superfine powders, high-purity magnesium oxide, activated magnesia, silicon-steel grade magnesium oxide, high-purity carbon
The important source material of sour magnesium, high-purity magnesite clinker, high-purity fused magnesite, magnesium oxide single-crystal, magnesia ceramics etc., can be widely applied to
The industries such as chemical industry, metallurgy, building materials, household electrical appliances, plastics, rubber, electronics, ceramics, and medicine, food.China is magnesium resource big country
But it not makes the country prosperous, there are many defects in production technology, product quality is not high, and market adaptability is poor, mostly in the form of crude product
Outside exporting country, to cause serious waste.Therefore, preparing one kind that high purity magnesium hydroxide product is the utilization of resources with light burnt powder has
Efficacious prescriptions formula.
Invention content
The object of the present invention is to provide a kind of methods that the molten light burnt powder of acid prepares high purity magnesium hydroxide, and this method is respectively with light
Burn powder, spent acid（Hydrochloric acid, nitric acid, sulfuric acid etc.）It is reaction mass for raw material, ammonia, by bubbling reactor that ammonia is direct
The magnesium salt solution for being passed through preparation is reacted, and room temperature one-step method prepares high-purity hydroxide under conditions of without using surfactant
The method of magnesium., process realization low using the method production cost is easy, product quality is high；It simultaneously can be from magnesium sinking by crystallization process
Filtrate obtains ammonium salt raw material and reaction product ammonia, so that reaction mass ammonia recycles, reaching reduces cost, reduces pollutant
The effect of discharge.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide, the method includes following preparation process：
Using light burnt powder as raw material, with waste acid liquor（Hydrochloric acid, nitric acid, sulfuric acid etc.）Mixing carries out the molten reaction of acid, it is molten that magnesium salts is made
Liquid obtains magnesium salts refined liquid using removal of impurities；The above solution is added in bubbling style reactor and is heated, precipitating reagent ammonia is then
It is passed into the form of bubbling in the reaction solution, reaction solution is aged through constant temperature, obtains high-purity hydrogen-oxygen after filtration washing and drying process
Change magnesium powder body；Reacted, ageing and filtration washing and drying process obtain magnesium hydrate powder, will be in filtrate by crystallization reaction
Magnesium precipitate of the Ammonia recovery for back react, the ammonium salt crystallization in solution is precipitated.
A kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide, the molten reaction of acid produce liquid and carry out preliminary sedimentation
It forms sediment, soluble impurity is further removed, to keep magnesium hydroxide products regular appearance, the size distribution of preparation uniform.
A kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide, the reactant ammonia is directly with bubbling
Mode enters reaction system and is reacted with magnesium salt solution, is settled out magnesium hydroxide products.
A kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide, the molten reaction temperature of acid are 20~80
DEG C, the reaction time is 1~3 h；Magnesium sinking reaction temperature is 60~100 DEG C, a concentration of 1~4 mol/L of magnesium salts refined liquid, reaction
Time is 2~6 h.
A kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide, the magnesium hydroxide products laser of the preparation
Particles distribution instrument tests average grain diameter D50It is 0.25~1.5 μm；XRD tests I001/I101It is 0.75~1.5.
Advantages of the present invention is with effect：
1. using ammonia for reaction mass, product mother liquor, which is filtered, washed, after reaction is easy, and magnesium hydroxide products purity is very high.
2. using bubbling bed reactor, ammonia is passed directly into magnesium salt solution by bubbling mode, to optimizing reaction system
Macroscopical and microcosmic mixed effect.
3. product particle crystal form obtained by is full, uniform and good dispersion, and specific surface area is less than the hexagonal flake with grain size
Particle（Octahedral structure）.Product particle epigranular（Narrow distribution range）, average grain diameter D50Less than 1.0 μm, the largest particles diameter
Less than 5.0 μm.
4. reaction is in relatively mild temperature（Less than 100 DEG C）And pressure（Essentially normal pressure）Condition is completed in next step, is not necessarily to
Hydro-thermal process need not use the auxiliary agent for adjusting the effect of product crystal form（Such as surface modifier）, operating procedure is simple, required to set
Standby easy to implement and floor space is few, and can be good at controlling diameter of particle distribution and crystal form.It does not use during the reaction
Surface modifier, to reduce production cost and external environmental.
5. ammonia can be recycled from product filtrate using crystallization process realizes that ammonia recycles, meanwhile, prepare ammonium salt product.Further
The economic benefit of the technique is improved, pollutant emission is reduced.
6. the technique that the present invention develops can acid extracting synthesize high quality fire retardant type MH products, operating procedure is simple, institute
Need equipment and floor space few, energy consumption is few, and equipment investment and producing cost are low, and pollutant discharge amount is few, are suitable for large-scale production.
Description of the drawings
Fig. 1 is magnesium hydrate powder grain shape photo；
Fig. 2 is magnesium hydroxide products particle characterization particle size distribution figure；
Fig. 3 is magnesium hydroxide products particle characterization XRD diagram.
Specific implementation mode
The present invention is by light burnt powder and spent acid（Hydrochloric acid, nitric acid, sulfuric acid etc.）Wiring solution-forming carries out the molten reaction of acid by a certain percentage
And filter, obtained magnesium salt solution, which is passed through a certain amount of ammonia, to be pre-processed and is filtered, finally will treated magnesium salt solution
It is added in bubbling style reactor, and ammonia is passed directly into a manner of being bubbled by certain gas liquid ratio in the case that being sufficiently stirred,
Controlling reaction temperature is in carrying out magnesium sinking reaction in a certain range, it is 7~10 or so to react certain time and reacting liquid pH value, constant temperature
It is filtered, washed and is dried to obtain loose high purity magnesium hydroxide powder after 1~4 h of ageing.Ammonium salt can be used for it in filtrate
His purposes, to which ammonia recycles.Magnesium sinking reaction in without using the auxiliary agents such as surfactant, sintetics without using
Water-heat process processing, to reducing production cost, reducing production stage and capable of realizing continuous process production.Filter out magnesium hydroxide
Filtrate after product can further carry out crystallization reaction with realize the ammonia of whole process recycle, the preparation of ammonium salt product.From
And reduce the consumption of ammonia, object discharge.
Embodiment one
The refined grain magnesium salt solution for configuring 1.0mol/L takes solution 500mL to be added in the bubbling style reactor that volume is 2000mL,
Ammonia is passed directly into the form of being bubbled to reaction solution and carries out magnesium sinking reaction, ammonia flow 500mL/min, 50 DEG C of isothermal reactions
2h reacting liquid pH values are 9.5 or so, obtain the milky suspension of magnesium hydroxide and ammonium salt.Product liquid after vacuum filtration ageing,
Filter cake is dried in vacuo 12h after being washed with deionized 3 times under the conditions of 80 DEG C, and it is micro- to obtain the good laxity bulk of crystallization degree
Thin magnesium hydrate powder.Filtrate returns to ammonia steaming device, and supplements appropriate magnesium source, circulate operation.
Embodiment two
With light burnt powder, spent acid（Hydrochloric acid, nitric acid, sulfuric acid etc.）It is molten that the magnesium salts that substance withdrawl syndrome is about 1.0mol/L is prepared for raw material
Liquid takes solution 500mL to be added in the bubbling style reactor that volume is 2000mL, solution and its temperature is controlled in stirred reactor
In 90 DEG C, ammonia is passed directly into reaction solution in the form of being bubbled and carries out magnesium sinking reaction, ammonia flow 500mL/min, 90 DEG C of perseverances
Temperature reaction 3h reacting liquid pH values are 9.5 or so, obtain the milky suspension of magnesium hydroxide and ammonium salt.70 DEG C of constant temperature of reaction mixture
It is aged 1h, product liquid after vacuum filtration ageing, filter cake is dried in vacuo 12h under the conditions of 80 DEG C after being washed with deionized 3 times, obtains
To the good laxity bulk high purity magnesium hydroxide powder of crystallization degree, average diameter of particles D50About 0.7 μm, maximum particle diameter
（Second particle）Less than 5.0 μm.
Claims (5)
1. a kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide, which is characterized in that prepared the method includes following
Journey：
Using light burnt powder as raw material, with waste acid liquor（Hydrochloric acid, nitric acid, sulfuric acid etc.）Mixing carries out the molten reaction of acid, it is molten that magnesium salts is made
Liquid obtains magnesium salts refined liquid using removal of impurities；The above solution is added in bubbling style reactor and is heated, precipitating reagent ammonia is then
It is passed into the form of bubbling in the reaction solution, reaction solution is aged through constant temperature, obtains high-purity hydrogen-oxygen after filtration washing and drying process
Change magnesium powder body；Reacted, ageing and filtration washing and drying process obtain magnesium hydrate powder, will be in filtrate by crystallization reaction
Magnesium precipitate of the Ammonia recovery for back react, the ammonium salt crystallization in solution is precipitated.
2. a kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide according to claim 1, which is characterized in that described
The molten reaction of acid produces liquid and carries out preformed precipitate, soluble impurity is further removed, to make the magnesium hydroxide products pattern of preparation advise
It is whole, size distribution is uniform.
3. a kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide according to claim 1, which is characterized in that described
Reactant ammonia is directly entered reaction system in a manner of bubbling and is reacted with magnesium salt solution, is settled out magnesium hydroxide products.
4. a kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide according to claim 1, which is characterized in that described
The molten reaction temperature of acid is 20~80 DEG C, and the reaction time is 1~3 h；Magnesium sinking reaction temperature is 60~100 DEG C, magnesium salts refined liquid
A concentration of 1~4 mol/L, reaction time are 2~6 h.
5. a kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide according to claim 1, which is characterized in that described
The magnesium hydroxide products laser fineness gage test average grain diameter D of preparation50It is 0.25~1.5 μm；XRD tests I001/I101
It is 0.75~1.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810562030.XA CN108502906A (en) | 2018-06-04 | 2018-06-04 | A kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide |
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| CN201810562030.XA CN108502906A (en) | 2018-06-04 | 2018-06-04 | A kind of method that the molten light burnt powder of acid prepares high purity magnesium hydroxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109721082A (en) * | 2019-03-22 | 2019-05-07 | 青海爱能森新材料科技有限公司 | A kind of production method of high purity magnesium hydroxide and potassium nitrate coproduction |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613108A (en) * | 2013-12-02 | 2014-03-05 | 沈阳化工大学 | Method for preparing magnesium hydroxide flame retardant by ammonia gas process |
| CN107758706A (en) * | 2017-09-25 | 2018-03-06 | 沈阳化工大学 | One-step method prepares cubic pieces flame retardant of magnesium hydroxide process |
-
2018
- 2018-06-04 CN CN201810562030.XA patent/CN108502906A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613108A (en) * | 2013-12-02 | 2014-03-05 | 沈阳化工大学 | Method for preparing magnesium hydroxide flame retardant by ammonia gas process |
| CN107758706A (en) * | 2017-09-25 | 2018-03-06 | 沈阳化工大学 | One-step method prepares cubic pieces flame retardant of magnesium hydroxide process |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109721082A (en) * | 2019-03-22 | 2019-05-07 | 青海爱能森新材料科技有限公司 | A kind of production method of high purity magnesium hydroxide and potassium nitrate coproduction |
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