CN109437259A - The continuous preparation method of magnesium hydroxide - Google Patents
The continuous preparation method of magnesium hydroxide Download PDFInfo
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- CN109437259A CN109437259A CN201811348716.5A CN201811348716A CN109437259A CN 109437259 A CN109437259 A CN 109437259A CN 201811348716 A CN201811348716 A CN 201811348716A CN 109437259 A CN109437259 A CN 109437259A
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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
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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Abstract
The present invention provides a kind of continuous preparation methods of magnesium hydroxide.This method comprises: step S1, magnesium ion solution will be contained and precipitating reagent carries out precipitation reaction, and persistently add during precipitation reaction it is fresh described in containing magnesium ion solution, obtain magnesium hydroxide slurry；Step S2 carries out precipitation reaction using a part in magnesium hydroxide slurry as being back in step S1 after crystal seed, with fresh precipitant mix；Wherein precipitating reagent is the mixture of alkali metal hydroxide and ammonium hydroxide.The magnesium hydroxide purity that above-mentioned preparation method obtains is higher, and sulphur, chlorinity are lower.Meanwhile the method can prepare magnesium hydroxide with serialization, improve into and produce efficiency, and crystal seed is added and also helps the particle diameter distribution and pattern for improving magnesium hydroxide, obtained magnesium hydroxide products particle diameter distribution is narrower, and pattern is mellow and full, close to spherical shape.
Description
Technical field
The present invention relates to technical field of preparation for inorganic material, in particular to a kind of continuous preparation side of magnesium hydroxide
Method.
Background technique
Magnesium hydroxide production at present substantially uses ammonia process and magnesium chloride lime method.
A kind of method that ammonia process prepares magnesium hydroxide is disclosed in Chinese patent CN107032374A, specifically by coal dust and
Ammonium chloride carries out displacement reaction, obtains magnesium chloride solution, recycles ammonium hydroxide and magnesium chloride solution to carry out precipitation reaction and obtains hydrogen-oxygen
Change magnesium.
A kind of method that lime method prepares magnesium hydroxide is disclosed in Chinese patent CN103601124A, it specifically will calcining
Quick lime afterwards, which is added into digestion medium, carries out digestion reaction generation milk of lime, then milk of lime is added molten to bischofite
It is reacted in liquid, obtains magnesium hydroxide.
However, due to the contaminant problems such as technology controlling and process and calcium, sulphur, the hydrogen-oxygen of above-mentioned ammonia process and the preparation of magnesium chloride lime method
It is not high to change magnesium products quality, sulphur, chlorinity are high, and broad particle distribution.
Summary of the invention
The main purpose of the present invention is to provide a kind of continuous preparation methods of magnesium hydroxide, to solve ammonia in the prior art
Method or the magnesium hydroxide sulphur of magnesium chloride lime method preparation, chlorinity are high, and the problem of broad particle distribution.
To achieve the goals above, according to an aspect of the invention, there is provided a kind of continuous preparation side of magnesium hydroxide
Method comprising: step S1 will contain magnesium ion solution and precipitating reagent carries out precipitation reaction, and continue during precipitation reaction
It adds fresh containing magnesium ion solution, obtains magnesium hydroxide slurry；Step S2, by a part in magnesium hydroxide slurry as brilliant
Kind, precipitation reaction is carried out with being back in step S1 after fresh precipitant mix；Wherein precipitating reagent is alkali metal hydroxide
With the mixture of ammonium hydroxide.
It further, is Adlerika containing magnesium ion solution, alkali metal hydroxide is sodium hydroxide and/or hydroxide
Potassium.
Further, the molar ratio of alkali metal hydroxide and ammonium hydroxide is 0.05~1:1.
Further, the temperature of precipitation reaction is 40~120 DEG C, and the reaction time is 1~5h.
Further, the hydrogen as precipitation reaction in the magnesium hydrate precipitate and step S1 in the magnesium hydroxide slurry of crystal seed
Weight ratio between magnesia production quantity is 0.5~8:1.
Further, during precipitation reaction, while to containing pattern controlling agent is added in magnesium ion solution, pattern is controlled
Agent is one of Tween-80, ethyl alcohol, polyethylene glycol, sodium alkyl benzene sulfonate, sodium alkyl sulfonate and sodium lignin sulfonate or more
Kind；Preferably, 0.5~3 gram of pattern controlling agent is added containing magnesium ion solution for every liter.
Further, the content containing magnesium ion in magnesium ion solution is 10~50g/L, preferably 25~35g/L.
Further, the molal quantity of hydroxide ion is 1 in the molal quantity and precipitating reagent containing magnesium ion in magnesium ion solution:
2~4.
Further, in step S1, precipitation reaction carries out while stirring, and stirring linear velocity is > 4m/s.
Further, in step S2, using a part in magnesium hydroxide slurry as crystal seed after, method further includes to surplus
The step of remaining magnesium hydroxide slurry is filtered, washs, drying to obtain magnesium hydroxide products；Preferably, in filtration step
The step of obtained filtrate carries out recovery ammonia processing, and preferably recovery ammonia is handled includes: to carry out causticization to filtrate using milk of lime, so
Filtering gypsum and ammonia still process afterwards obtain recycling ammonium hydroxide.
The present invention provides a kind of continuous preparation methods of magnesium hydroxide comprising: step S1, will contain magnesium ion solution with
Precipitating reagent carries out precipitation reaction, and persistently add during precipitation reaction it is fresh described in containing magnesium ion solution, obtain hydrogen
Magnesia slurry；Step S2, using a part in magnesium hydroxide slurry as being back to after crystal seed, with fresh precipitant mix
Precipitation reaction is carried out in step S1；Wherein precipitating reagent is the mixture of alkali metal hydroxide and ammonium hydroxide.
Above-mentioned preparation method provided by the invention is obtained using the mixture of alkali metal hydroxide and ammonium hydroxide as precipitating reagent
The magnesium hydroxide purity arrived is higher, and sulphur, chlorinity are lower.It, will be in magnesium hydroxide slurry meanwhile during precipitation reaction
A part is returned as crystal seed and precipitating reagent, to precipitate to fresh containing magnesium ion solution.It so both can be with serialization system
Standby magnesium hydroxide, improves into and produces efficiency, and crystal seed is added and also helps the particle diameter distribution and pattern for improving magnesium hydroxide, obtains
Magnesium hydroxide products particle diameter distribution is narrower, and pattern is mellow and full, close to spherical shape.
In short, can continuously prepare the higher magnesium hydroxide products of quality using above-mentioned preparation method, have extensive
Application prospect.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.Below in conjunction with embodiment, the present invention will be described in detail.
The application is described in further detail below in conjunction with specific embodiment, these embodiments should not be understood as limitation originally
Apply for range claimed.
As described in background technology part, in the prior art using ammonia process or the hydroxide of magnesium chloride lime method preparation
Magnesium, sulphur, chlorinity are high, and broad particle distribution.
To solve the above-mentioned problems, the present invention provides a kind of continuous preparation methods of magnesium hydroxide comprising: step
S1 will contain magnesium ion solution and precipitating reagent and carry out precipitation reaction, and persistently add during precipitation reaction fresh containing magnesium
Solion obtains magnesium hydroxide slurry；Step S2 sinks using a part in magnesium hydroxide slurry as crystal seed with fresh
It is back in step S1 after shallow lake agent mixing and carries out precipitation reaction；Wherein precipitating reagent is the mixing of alkali metal hydroxide and ammonium hydroxide
Object.
Above-mentioned preparation method provided by the invention is obtained using the mixture of alkali metal hydroxide and ammonium hydroxide as precipitating reagent
The magnesium hydroxide purity arrived is higher, and sulphur, chlorinity are lower.It, will be in magnesium hydroxide slurry meanwhile during precipitation reaction
A part is returned as crystal seed and precipitating reagent, to precipitate to fresh containing magnesium ion solution.It so both can be with serialization system
Standby magnesium hydroxide, improves into and produces efficiency, and crystal seed is added and also helps the particle diameter distribution and pattern for improving magnesium hydroxide, obtains
Magnesium hydroxide products particle diameter distribution is narrower, and pattern is mellow and full, close to spherical shape.
In short, can continuously prepare the higher magnesium hydroxide products of quality using above-mentioned preparation method, have extensive
Application prospect.
It is sulphur containing magnesium ion solution in a preferred embodiment to further increase the quality of magnesium hydroxide
Sour magnesium solution, alkali metal hydroxide are sodium hydroxide and/or potassium hydroxide；It is highly preferred that alkali metal hydroxide and ammonium hydroxide
Molar ratio be 0.05~1:1.
In a preferred embodiment, the temperature of precipitation reaction is 40~120 DEG C, and the reaction time is 1~5h.At this
At a temperature of carry out precipitation reaction, can further improve the pattern of magnesium hydroxide products and pure while improving reaction efficiency
Degree.
In above-mentioned steps S2, contain magnesium hydrate precipitate in the magnesium hydroxide slurry of return, this partly precipitated is passed through fresh
Containing crystal seed is used as in magnesium ion solution, new being deposited on crystal seed can be promoted to grow up, form the good magnesium hydroxide of pattern
Precipitating.In a preferred embodiment, as in the magnesium hydrate precipitate and step S1 in the magnesium hydroxide slurry of crystal seed
Weight ratio between the magnesium hydroxide production quantity of precipitation reaction is 0.5~8:1.The additive amount of crystal seed is controlled in above range,
Be conducive to further promote growing up for magnesium hydroxide, while being conducive to that excessive crystal seed is avoided to reduce magnesium hydroxide production efficiency,
Or be conducive to the settling velocity for avoiding very few crystal seed from influencing magnesium hydroxide.And the crystal seed of the above-mentioned dosage of addition also can be further
Improve the pattern of magnesium hydroxide, and keeps its particle diameter distribution more uniform.
In a preferred embodiment, during precipitation reaction, while pattern is added to containing in magnesium ion solution
Controlling agent, pattern controlling agent are Tween-80, ethyl alcohol, polyethylene glycol, sodium alkyl benzene sulfonate, sodium alkyl sulfonate and lignin sulfonic acid
One of sodium is a variety of.These reagents are added and are more advantageous to the pattern for improving magnesium hydroxide, keep it more mellow and fuller, are formed spherical
Particle.Preferably, 0.5~3 gram of pattern controlling agent is added containing magnesium ion solution for every liter.
In order to further increase the production efficiency and quality of magnesium hydroxide, in a preferred embodiment, containing magnesium from
The content of magnesium ion is 10~50g/L, preferably 25~35g/L in sub- solution.It is highly preferred that containing magnesium ion in magnesium ion solution
Molal quantity and precipitating reagent in hydroxide ion molal quantity be 1:2~4.
In a preferred embodiment, in step S1, precipitation reaction carries out while stirring, and stirs linear speed
Degree is > 4m/s.
In a preferred embodiment, in step S2, using a part in magnesium hydroxide slurry as crystal seed after,
Method further includes the steps that being filtered remaining magnesium hydroxide slurry, washs, dries to obtain magnesium hydroxide products.It is preferred that
The step of ground, filtrate obtained in filtration step carry out recovery ammonia processing, and preferably recovery ammonia is handled includes: using milk of lime to filter
Liquid carries out causticization, then filters gypsum and ammonia still process, obtains recycling ammonium hydroxide.Be conducive to resource recycling in this way, what ammonia still process generated
Ammonium hydroxide can be further used for configuring precipitating reagent.Waste water after ammonia still process after processing can be with direct emission.
Beneficial effects of the present invention are further illustrated by the following examples:
Embodiment 1
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: ammonium hydroxide (mol) 0.1:1 is as precipitating reagent (mole of magnesium ion
Several molal quantitys with hydroxide ion in precipitating reagent are 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 4:1, are added
Ethyl alcohol 1g/L, stir linear velocity 5m/s, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is spherical shape, and 10 μm of D50, partial size is 10 ± 2 μm, sulfur content 0.1wt%, and chlorinity is
0.The process magnesium rate of recovery > 95%.
Embodiment 2
Magnesium sulfate stoste 1L, 30g/L containing magnesium, potassium hydroxide: ammonium hydroxide (mol) 0.1:1 is as precipitating reagent (mole of magnesium ion
Several molal quantitys with hydroxide ion in precipitating reagent are 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 4:1, are added
Ethyl alcohol 1g/L, stir linear velocity 5m/s, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is spherical shape, and 11 μm of D50, partial size is 11 ± 4 μm, sulfur content 0.08wt%, chlorinity
It is 0.The process magnesium rate of recovery > 94%.
Embodiment 3
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: as precipitating reagent, (magnesium ion rubs ammonium hydroxide (mol) 0.05:1
Reflux crystal seed is added for 1:3) by the molal quantity of number and hydroxide ion in precipitating reagent in you, and crystal seed and product production quantity ratio are 4:1, are added
Enter ethyl alcohol 1g/L, stirs linear velocity 5m/s, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is spherical shape, and 10 μm of D50, partial size is 10 ± 3 μm, sulfur content 0.1wt%, and chlorinity is
0.The process magnesium rate of recovery > 96%.
Embodiment 4
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: ammonium hydroxide (mol) 1:1 is as the precipitating reagent (molal quantity of magnesium ion
Molal quantity with hydroxide ion in precipitating reagent is 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 4:1, and second is added
Alcohol 1g/L, stir linear velocity 5m/s, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is spherical shape, and 10 μm of D50, partial size is 10 ± 4 μm, sulfur content 0.12wt%, chlorinity
It is 0.The process magnesium rate of recovery > 95%.
Embodiment 5
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: as precipitating reagent, (magnesium ion rubs ammonium hydroxide (mol) 0.03:1
Reflux crystal seed is added for 1:3) by the molal quantity of number and hydroxide ion in precipitating reagent in you, and crystal seed and product production quantity ratio are 4:1, are added
Enter ethyl alcohol 1g/L, stirs linear velocity 5m/s, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is spherical shape, and 9 μm of D50, partial size is 9 ± 4 μm, sulfur content 0.14wt%, and chlorinity is
0.The process magnesium rate of recovery > 93%.
Embodiment 6
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: ammonium hydroxide (mol) 0.1:1 is as precipitating reagent (mole of magnesium ion
Several molal quantitys with hydroxide ion in precipitating reagent are 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 4:1, are added
Ethyl alcohol 1g/L, stir linear velocity 5m/s, 40 DEG C of precipitation temperature, sedimentation time 5h.
Through analyzing after suction filtration, product is spherical shape, and 10 μm of D50, partial size is 10 ± 3 μm, sulfur content 0.09wt%, chlorinity
It is 0.The process magnesium rate of recovery > 95%.
Embodiment 7
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: ammonium hydroxide (mol) 0.1:1 is as precipitating reagent (mole of magnesium ion
Several molal quantitys with hydroxide ion in precipitating reagent are 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 4:1, are added
Ethyl alcohol 1g/L, stir linear velocity 5m/s, 120 DEG C of precipitation temperature, sedimentation time 1h.
Through analyzing after suction filtration, product is spherical shape, and 8 μm of D50, partial size is 8 ± 3 μm, sulfur content 0.12wt%, and chlorinity is
0.The process magnesium rate of recovery > 94%.
Embodiment 8
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: ammonium hydroxide (mol) 0.1:1 is as precipitating reagent (mole of magnesium ion
Several molal quantitys with hydroxide ion in precipitating reagent are 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 4:1, are added
Ethyl alcohol 1g/L, stir linear velocity 5m/s, 35 DEG C of precipitation temperature, sedimentation time 5h.
Through analyzing after suction filtration, product is spherical shape, and 9 μm of D50, partial size is 9 ± 5 μm, sulfur content 0.14wt%, and chlorinity is
0.The process magnesium rate of recovery > 95%.
Embodiment 9
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: ammonium hydroxide (mol) 0.1:1 is as precipitating reagent (mole of magnesium ion
Several molal quantitys with hydroxide ion in precipitating reagent are 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 0.5:1, are added
Enter ethyl alcohol 1g/L, stirs linear velocity 5m/s, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is spherical shape, and 8 μm of D50, partial size is 8 ± 3 μm, sulfur content 0.13wt%, and chlorinity is
0.The process magnesium rate of recovery > 93%.
Embodiment 10
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: ammonium hydroxide (mol) 0.1:1 is as precipitating reagent (mole of magnesium ion
Several molal quantitys with hydroxide ion in precipitating reagent are 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 8:1, are added
Ethyl alcohol 1g/L, stir linear velocity 5m/s, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is spherical shape, and 12 μm of D50, partial size is 12 ± 5 μm, sulfur content 0.09wt%, chlorinity
It is 0.The process magnesium rate of recovery > 95%.
Embodiment 11
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: ammonium hydroxide (mol) 0.1:1 is as precipitating reagent (mole of magnesium ion
Several molal quantitys with hydroxide ion in precipitating reagent are 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 0.2:1, are added
Enter ethyl alcohol 1g/L, stirs linear velocity 5m/s, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is spherical shape, and 7 μm of D50, partial size is 7 ± 2 μm, sulfur content 0.15wt%, and chlorinity is
0.The process magnesium rate of recovery > 92%.
Embodiment 12
Magnesium chloride stoste 1L, 30g/L containing magnesium, sodium hydroxide: ammonium hydroxide (mol) 0.1:1 is as precipitating reagent (mole of magnesium ion
Several molal quantitys with hydroxide ion in precipitating reagent are 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 4:1, are added
Ethyl alcohol 1g/L, stir linear velocity 5m/s, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is spherical shape, and 11 μm of D50, partial size is 11 ± 3 μm, and sulfur content is that chlorinity is
0.05wt%.The process magnesium rate of recovery > 96%.
Embodiment 13
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: ammonium hydroxide (mol) 0.1:1 is as precipitating reagent (mole of magnesium ion
Several molal quantitys with hydroxide ion in precipitating reagent are 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 4:1, are added
Tween-80 1g/L, stir linear velocity 5m/s, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is spherical shape, and 11 μm of D50, partial size is 11 ± 3 μm, sulfur content 0.11wt%, chlorinity
It is 0.The process magnesium rate of recovery > 95%.
Embodiment 14
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: ammonium hydroxide (mol) 0.1:1 is as precipitating reagent (mole of magnesium ion
Several molal quantitys with hydroxide ion in precipitating reagent are 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 4:1, are added
Ethyl alcohol 0.5g/L, stir linear velocity 5m/s, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is spherical shape, and 12 μm of D50, partial size is 12 ± 5 μm, sulfur content 0.11wt%, chlorinity
It is 0.The process magnesium rate of recovery > 95%.
Embodiment 15
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: ammonium hydroxide (mol) 0.1:1 is as precipitating reagent (mole of magnesium ion
Several molal quantitys with hydroxide ion in precipitating reagent are 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 4:1, are added
Ethyl alcohol 3g/L, stir linear velocity 5m/s, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is spherical shape, and 11 μm of D50, partial size is 11 ± 3 μm, sulfur content 0.1wt%, and chlorinity is
0.The process magnesium rate of recovery > 96%.
Comparative example 1
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide: ammonium hydroxide (mol) 0.1:1 is as precipitating reagent (mole of magnesium ion
Several molal quantitys with hydroxide ion in precipitating reagent are 1:3), do not flow back crystal seed, and ethyl alcohol 1g/L is added, and stirs linear velocity 5m/
S, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is elliposoidal, and D50 5um, partial size is 5 ± 4 μm, sulfur content 0.4wt%, and chlorinity is
0.The process magnesium rate of recovery > 90%.
Comparative example 2
Magnesium sulfate stoste 1L, 30g/L containing magnesium, sodium hydroxide is as precipitating reagent (hydrogen in the molal quantity and precipitating reagent of magnesium ion
The molal quantity of oxygen radical ion is 1:3) reflux crystal seed is added, crystal seed and product production quantity ratio are 4:1, and ethyl alcohol 1g/L, stirring is added
Linear velocity 5m/s, 65 DEG C of precipitation temperature, sedimentation time 4h.
Through analyzing after suction filtration, product is elliposoidal, and 10 μm of D50, partial size is 10 ± 6 μm, sulfur content 0.3wt%, chlorinity
It is 0.The process magnesium rate of recovery > 90%.
It can be seen from the above description that the above embodiments of the present invention realized the following chievements:
Above-mentioned preparation method provided by the invention is obtained using the mixture of alkali metal hydroxide and ammonium hydroxide as precipitating reagent
The magnesium hydroxide purity arrived is higher, and sulphur, chlorinity are lower.It, will be in magnesium hydroxide slurry meanwhile during precipitation reaction
A part is returned as crystal seed and precipitating reagent, to precipitate to fresh containing magnesium ion solution.It so both can be with serialization system
Standby magnesium hydroxide, improves into and produces efficiency, and crystal seed is added and also helps the particle diameter distribution and pattern for improving magnesium hydroxide, obtains
Magnesium hydroxide products particle diameter distribution is narrower, and pattern is mellow and full, close to spherical shape.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of continuous preparation method of magnesium hydroxide, which is characterized in that the described method includes:
Step S1, will contain magnesium ion solution and precipitating reagent carries out precipitation reaction, and persistently add during the precipitation reaction
Add fresh described containing magnesium ion solution, obtains magnesium hydroxide slurry；
Step S2, using a part in the magnesium hydroxide slurry as being returned after crystal seed, with the fresh precipitant mix
The precipitation reaction is carried out in the extremely step S1；
Wherein the precipitating reagent is the mixture of alkali metal hydroxide and ammonium hydroxide.
2. the method according to claim 1, wherein the magnesium ion solution that contains is Adlerika, the alkali
Metal hydroxides is sodium hydroxide and/or potassium hydroxide.
3. the method according to claim 1, wherein the molar ratio of the alkali metal hydroxide and the ammonium hydroxide
For 0.05~1:1.
4. according to the method in any one of claims 1 to 3, which is characterized in that the temperature of the precipitation reaction be 40~
120 DEG C, the reaction time is 1~5h.
5. method according to claim 1 to 4, which is characterized in that the hydroxide as the crystal seed
Weight ratio in magnesium hydrate precipitate and the step S1 in magnesium slurry between the magnesium hydroxide production quantity of precipitation reaction is 0.5
~8:1.
6. according to the method described in claim 5, it is characterized in that, during the precipitation reaction, while containing magnesium to described
In solion be added pattern controlling agent, the pattern controlling agent be Tween-80, ethyl alcohol, polyethylene glycol, sodium alkyl benzene sulfonate,
One of sodium alkyl sulfonate and sodium lignin sulfonate are a variety of；
Preferably, 0.5~3 gram of pattern controlling agent is added containing magnesium ion solution described in every liter.
7. method according to any one of claim 1 to 6, which is characterized in that described containing magnesium ion in magnesium ion solution
Content be 10~50g/L, preferably 25~35g/L.
8. the method according to the description of claim 7 is characterized in that the molal quantity and institute containing magnesium ion in magnesium ion solution
The molal quantity for stating hydroxide ion in precipitating reagent is 1:2~4.
9. method according to any one of claim 1 to 6, which is characterized in that in the step S1, the precipitation reaction
It carries out while stirring, and stirring linear velocity is > 4m/s.
10. method according to any one of claim 1 to 6, which is characterized in that in the step S2, by the hydrogen-oxygen
After changing a part in magnesium slurry as crystal seed, the method also includes carrying out to the remaining magnesium hydroxide slurry
The step of filter, washing, drying are to obtain magnesium hydroxide products；
Preferably, the step of filtrate obtained in the filtration step carries out recovery ammonia processing, and preferably the recovery ammonia is handled is wrapped
It includes: causticization being carried out to the filtrate using milk of lime, then filters gypsum and ammonia still process, obtains recycling ammonium hydroxide.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110655093A (en) * | 2019-11-19 | 2020-01-07 | 中国科学院过程工程研究所 | A kind of preparation method of ultrafine magnesium hydroxide |
| CN114560478A (en) * | 2022-02-22 | 2022-05-31 | 西安交通大学 | A kind of raw salt refining method and system |
| CN114735728A (en) * | 2022-04-19 | 2022-07-12 | 广西南宁百会药业集团有限公司 | Preparation method and application of magnesium hydroxide |
| CN116514149A (en) * | 2023-05-16 | 2023-08-01 | 自然资源部天津海水淡化与综合利用研究所 | A kind of preparation method of florescent magnesium hydroxide taking magnesium oxide as raw material |
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| CN101760641A (en) * | 2008-12-24 | 2010-06-30 | 中国恩菲工程技术有限公司 | Technology for recovering magnesium from magnesium sulfate solution |
| KR20130008895A (en) * | 2011-07-13 | 2013-01-23 | 일솜 주식회사 | Apparatus for preparing magnesium hydroxide from bitterns |
| CN102807238A (en) * | 2012-08-24 | 2012-12-05 | 中国科学院青海盐湖研究所 | Method for preparing spherical magnesium hydroxide |
| CN102849761A (en) * | 2012-09-30 | 2013-01-02 | 河北工业大学 | Preparation method of magnesium hydrate |
| CN105060320A (en) * | 2015-07-23 | 2015-11-18 | 韦海棉 | Method for preparing magnesium hydroxide by high magnesium-lithium ratio salt lake brine |
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| CN110655093A (en) * | 2019-11-19 | 2020-01-07 | 中国科学院过程工程研究所 | A kind of preparation method of ultrafine magnesium hydroxide |
| CN114560478A (en) * | 2022-02-22 | 2022-05-31 | 西安交通大学 | A kind of raw salt refining method and system |
| CN114735728A (en) * | 2022-04-19 | 2022-07-12 | 广西南宁百会药业集团有限公司 | Preparation method and application of magnesium hydroxide |
| CN114735728B (en) * | 2022-04-19 | 2024-01-26 | 广西南宁百会药业集团有限公司 | Preparation method and application of magnesium hydroxide |
| CN116514149A (en) * | 2023-05-16 | 2023-08-01 | 自然资源部天津海水淡化与综合利用研究所 | A kind of preparation method of florescent magnesium hydroxide taking magnesium oxide as raw material |
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