CN107572565A - The method and apparatus that a kind of pipe reaction continuously prepares magnesium hydroxide - Google Patents
The method and apparatus that a kind of pipe reaction continuously prepares magnesium hydroxide Download PDFInfo
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- CN107572565A CN107572565A CN201710752426.6A CN201710752426A CN107572565A CN 107572565 A CN107572565 A CN 107572565A CN 201710752426 A CN201710752426 A CN 201710752426A CN 107572565 A CN107572565 A CN 107572565A
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- magnesium hydroxide
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Abstract
The present invention relates to the preparing technical field of magnesium hydroxide, and in particular to a kind of method and apparatus that magnesium hydroxide is prepared by pipe reaction.Traditional magnesium hydroxide production uses tank reactor, the shortcomings of product cut size span is big, and residual chlorine is high, product quality difference be present.Although there is technology to propose some improvement, the shortcomings of introducing auxiliary agent increase cost be present.Technical scheme provided by the invention is：Magnesium salt solution and raw material containing ammonia after quick mixing, are passed through the tubular reactor control condition such as temperature and pH and reacted in super mixer.Because tubular reactor reduces the back-mixing and parcel of material, so that the magnesium hydroxide products particle size span prepared is small, pattern is unified, and residual chlorine is low.Present invention also offers the device for implementing the technical scheme, its structure includes pump supply unit, Hi-mixer, tubular reactor and the product filter element being linked in sequence.The method of the invention and device are applied to the industrial production of magnesium hydroxide.
Description
Technical field
The present invention relates to the preparing technical field of magnesium hydroxide, and in particular to a kind of pipe reaction prepares the side of magnesium hydroxide
Method and device.
Background technology
Magnesium hydroxide is widely used in flue gas desulfurization and sewage disposal as a kind of basic chemical industry raw material.Magnesium hydroxide conduct
A kind of new inorganic combustion inhibitor, itself is nonpoisonous and tasteless, and toxic gas will not be not only produced in decomposable process, and due to it certainly
The alkalescence of body, it can also be neutralized with caused deleterious acidic gas in combustion process, reduce environmental pollution, be received by the market.
And China there are the premier magnesium ore resources in the world, enough guarantees are provided for the development of magnesium hydroxide.
In traditional magnesium hydroxide production, using still reaction, continuous production is realized by interval or multi-floating bodies, it is lacked
Point is that product cut size span is big, and residual chlorine is high, and product quality is poor.In the prior art, patent document CN200910011079.7 is proposed
A kind of method that ammonia synthesizes magnesium hydroxide by bubbling reactor, realized by the method for adding surfactant than tradition
The more preferable size controlling of method；Patent CN201010507480.2 has invented realizes that serialization prepares hydrogen-oxygen with supergravity reactor
Change the apparatus and method of magnesium, the shortcomings that internal circulating load is larger, and energy consumption is higher be present；Patent CN201310038980.X, which is proposed, to be passed through
The method that quick hybrid reaction is realized in injection reaction, and realize that not adding surfactant can also better control over than conventional method
Particle diameter.More than each inventive method all realize the circulation and stirring of material by still reaction, still inevitable material back mixing and
Parcel, causes that product cut size span is big, and topographical difference is larger, although proposing some improvement, exist introduce protective agent and plus
The shortcomings of big energy consumption.
The content of the invention
Using tank reactor to prepare product cut size span existing for magnesium hydroxide big for above-mentioned, topographical difference it is larger and
The problem of residual chlorine is high, the present invention provide a kind of method that pipe reaction continuously prepares magnesium hydroxide.The inventive method is using efficiently
The quick mixed reaction solution of blender and tubular reactor do not have the characteristics of reaction mass back-mixing and parcel, realize product grain
Footpath span is small, and pattern is unified, and residual chlorine is low, high as the magnesium hydroxide activity of raw material production using it.
It is a further object of the present invention to provide a kind of dress realized the pipe reaction and continuously prepare the method for magnesium hydroxide
Put.
The technical solution adopted by the present invention is as follows：
A kind of method that pipe reaction continuously prepares magnesium hydroxide, comprises the following steps：
[1] magnesium salt solution and raw material containing ammonia are inputted into Hi-mixer respectively quickly to be mixed, reacts and wrapped
Reaction solution containing magnesium hydroxide；
[2] by step [1] reaction solution out of Hi-mixer input tubular reactor, the tubular reactor
Constant temperature, pH are maintained 8.0-12.0；The reaction solution stops 3-30 minutes in the tubular reactor；
[3] reacting liquid filtering for obtaining step [2], obtains magnesium hydroxide products and reaction mother liquor.
Using this technical scheme, the back-mixing of material and parcel are reduced in tubular reactor, can be obtained without adding auxiliary agent
To the unified magnesium hydroxide products low with residual chlorine of product cut size pattern.
Preferably, the concentration of the magnesium salt solution is 0.5-4mol/L.The magnesium salt solution of the concentration range reacts life
During magnesium hydroxide, nucleus structure and uniform particle diameter that nucleation stage is formed, therefore the magnesium hydroxide production of final production
The grain diameter and pattern of product can be controlled effectively.
Preferably, the raw material containing ammonia is percent by volume 10%-99.9% gas ammonia, industrial ammonia or the step
[3] one or more combinations in the ammonia solution that the reaction mother liquor obtained in is configured to.The selection of the raw material containing ammonia is enriched, especially
It is that wherein remaining ammonia, energy-saving ring can be recycled with the reaction mother liquor after product is filtered in Selection utilization present invention process
Protect.
It is further preferred that step [1] magnesium salt solution and raw material containing ammonia are well mixed used in Hi-mixer
Time be less than 0.5-1s.Quick hybrid reaction material is advantageous to fast nucleation, further improves the equal of nucleus structure and particle diameter
One property, so as to further improve the homogeneity of the grain diameter of magnesium hydroxide products and pattern.
It is a kind of realize described in pipe reaction continuously prepare magnesium hydroxide method device, according to the flowing side of logistics
To device includes pump supply unit, Hi-mixer, tubular reactor and the product filter element being linked in sequence；The tubular type
Reactor is provided with heat exchanger, and the tubular reactor outlet is provided with online pH.
The method that pipe reaction provided by the invention continuously prepares magnesium hydroxide can be realized using the present apparatus.Described device
Production can be carried out continuously, reduce device volume and investment, operating cost is low, and device is safeguarded simply, improves production effect
Rate, by improving automaticity, reduce influence of the human factor to production；Pump supply unit can adjust material conveying
Amount, realizes being precisely controlled for reaction, so as to improve product quality and yield, and realizes the production of the product of plurality of specifications.
Preferably, the outlet of the tubular reactor is connected with accumulator still, the accumulator still outlet and product filter element
Connection.Addition accumulator still can buffer the pressure oscillation in reaction system, make Flow of Goods and Materials more steady.
Preferably, the product filtration unit outlet is connected with Recycling Mother Solution pump, the Recycling Mother Solution pump discharge with it is described
Pump circulation unit connects.Adding Recycling Mother Solution pump can make the reaction mother liquor after filtering flow directly into pump supply unit, make reaction
The recycling of mother liquor is simply efficient.
It is further preferred that the Hi-mixer is static mixer or dynamic mixer.Reaction mass can be improved
Mixing velocity, be advantageous to fast nucleation, nucleus structure and the homogeneity of particle diameter improved, so as to improve the particle of magnesium hydroxide products
The homogeneity of particle diameter and pattern.
It is further preferred that the static mixer is SV static mixers, SX static mixers or SK static mixers
In one or more combinations.It can further improve the mixing velocity of reaction mass.Further improve nucleus structure and particle diameter
Homogeneity, so as to further improve magnesium hydroxide products grain diameter and pattern homogeneity.
Compared with prior art, pipe reaction provided by the present invention continuously prepares the beneficial effect of the method for magnesium hydroxide
It is：The back-mixing of material and parcel are reduced in tubular reactor, and it is unified and residual to obtain product cut size pattern without addition auxiliary agent
The low magnesium hydroxide products of chlorine；Quick hybrid reaction material is advantageous to fast nucleation, further improves nucleus structure and particle diameter
Homogeneity, so as to further improve the homogeneity of the grain diameter of magnesium oxide product and pattern；The selection of the raw material containing ammonia is enriched, special
It is not that wherein remaining ammonia can be recycled with the reaction mother liquor after product is filtered in Selection utilization present invention process, energy-conservation
Environmental protection.
Compared with prior art, the method that the pipe reaction described in realization provided by the present invention continuously prepares magnesium hydroxide
The beneficial effect of device be：Production can be carried out continuously, reduce device volume and investment, operating cost is low, device dimension
Shield is simple, improves production efficiency, by improving automaticity, reduces influence of the human factor to production；Pump conveying is single
Member can adjust material conveying capacity, realize being precisely controlled for reaction, so as to improve product quality and yield, and realize plurality of specifications
Product production.
Embodiment
The present invention is further explained with reference to specific embodiment, will be described the optimal specific real of the present invention
Apply mode.
Embodiment 1
The magnesium chloride solution for using bischofite to be configured to and gas ammonia are reacted for raw material, and tubular reactor caliber DN50 is high
Effect blender is arranged to SX static mixers and SK static mixers.Tubular reactor is arranged to water cooling sleeve pipe, and magnesium chloride is molten
Preheater is set on liquid and industrial ammonia conveyance conduit.
Bischofite is configured to 2mol/L solution, it is 2m to open magnesium chloride feed pump and control flow3/ h, while open and add
The gas ammonia of pressure mixes in Hi-mixer, and it is 9.3- that the online pH set is exported using tubular reactor and controls reaction system pH
10.0, it is 40-60 DEG C using chuck water flowing cooling controlling reaction temperature, residence time 3-4min.Leave tubular reactor
Material enters accumulator still, then enters plate and frame filter press and is filtered, post-treated product perchloro-≤0.1wt%, D50 1.8-
2.2um,D100≤8um。
Embodiment 2
The magnesium chloride solution for using bischofite to be configured to and industrial ammonia are reacted for raw material, and reactor caliber DN50 is high
Effect blender is arranged to SV static mixers and SX static mixers, and tubular reactor is arranged to water cooling sleeve pipe, and magnesium chloride is molten
Preheater is set on liquid and industrial ammonia conveyance conduit.
Bischofite is configured to 4mol/L solution, it is 1m to open magnesium chloride feed pump and control flow3/ h, while open work
Industry ammoniacal liquor feed pump is mixed in Hi-mixer, and the online pH set is exported using tubular reactor and controls the reaction system pH to be
9.3-10.0, chuck water flowing cooling controlling reaction temperature is 40-60 DEG C, residence time 5-6min.Leave the material of reactor
Into accumulator still, then enter plate and frame filter press and filtered, post-treated product perchloro-≤0.1wt%, D50 1.8-
2.2um,D100≤8um。
Embodiment 3
Reaction use the magnesium chloride solution that bischofite is configured to and gas ammonia as raw material, first by gas ammonia with reacting mother during reaction
Liquid enters reactor again after absorbing into ammoniacal liquor.Reactor caliber DN50, Hi-mixer is arranged to SV static mixers and SX is static
Blender.Tubular reactor is arranged to water cooling sleeve pipe, and preheater is set on magnesium chloride solution and industrial ammonia conveyance conduit.
Bischofite is configured to 4mol/L solution, it is 1.0m to open Recycling Mother Solution pump and control flow3/ h, and open gas
Ammonia enters reaction system；Opening magnesium chloride feed pump simultaneously controls flow to be reacted for 1.0m3/h, makes reaction mass efficient
Mixed in blender, it is 9.3-10.0 that the online pH set is exported using tubular reactor and controls reaction system pH, utilizes chuck
Water flowing cooling controlling reaction temperature is 40-60 DEG C, residence time 5-6min.The material for leaving reactor enters accumulator still, so
Laggard plate and frame filter press is filtered, post-treated product perchloro-≤0.1wt%, D50 1.8-2.2um, D100≤8um.
Embodiment described above only expresses the embodiment of the application, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the application protection domain can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, on the premise of technical scheme design is not departed from, various modifications and improvements can be made, these belong to this
The protection domain of application.
Claims (9)
1. a kind of method that pipe reaction continuously prepares magnesium hydroxide, it is characterised in that the described method comprises the following steps：
[1] magnesium salt solution and raw material containing ammonia are inputted into Hi-mixer respectively quickly to be mixed, reacts to obtain and include hydrogen
The reaction solution of magnesia；
[2] step [1] reaction solution is inputted into tubular reactor from the Hi-mixer, it is permanent in the tubular reactor
Temperature, pH are maintained 8.0-12.0；The reaction solution stops 3-30 minutes in the tubular reactor；
[3] reacting liquid filtering for obtaining step [2], obtains magnesium hydroxide products and reaction mother liquor.
2. the method for magnesium hydroxide is continuously prepared according to the pipe reaction described in claim 1, it is characterised in that：The magnesium salts is molten
The concentration of liquid is 0.5-4mo l/L.
3. the method for magnesium hydroxide is continuously prepared according to the pipe reaction described in claim 1, it is characterised in that：It is described former containing ammonia
What the reaction mother liquor for expecting to obtain in the gas ammonia for percent by volume 10%-99.9%, industrial ammonia or the step [3] was configured to
One or more combinations in ammonia solution.
4. the method for continuously preparing magnesium hydroxide according to the pipe reaction described in claim any one of 1-3, it is characterised in that：Step
Suddenly [1] described magnesium salt solution and raw material containing ammonia well mixed time used in Hi-mixer are less than 0.5-1s.
5. a kind of pipe reaction realized described in claim 1 continuously prepares the device of the method for magnesium hydroxide, it is characterised in that：
Described device includes pump supply unit, Hi-mixer, tubular reactor and the product filter element being linked in sequence；The tubular type
Reactor is provided with heat exchanger, and the tubular reactor outlet is provided with online pH.
6. according to the device described in claim 5, it is characterised in that：The outlet of the tubular reactor is connected with accumulator still, institute
Accumulator still outlet is stated to be connected with product filter element.
7. according to the device described in claim 5, it is characterised in that：The product filtration unit outlet is connected with Recycling Mother Solution
Pump, the Recycling Mother Solution pump discharge are connected with the pump supply unit.
8. according to the device described in claim any one of 5-7, it is characterised in that：The Hi-mixer be static mixer or
Dynamic mixer.
9. according to the device described in claim 8, it is characterised in that：The static mixer is SV static mixers, SX static state
One or more combinations in blender or SK static mixers.
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| CN201710752426.6A CN107572565A (en) | 2017-08-28 | 2017-08-28 | The method and apparatus that a kind of pipe reaction continuously prepares magnesium hydroxide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110092408A (en) * | 2019-05-12 | 2019-08-06 | 广东工业大学 | A kind of method of continuous production copper oxide |
| CN112320827A (en) * | 2020-10-10 | 2021-02-05 | 沈阳化工大学 | Process for preparing magnesium hydroxide by cyclic reaction |
| CN112537787A (en) * | 2020-12-01 | 2021-03-23 | 沈阳化工大学 | Magnesium hydroxide continuous production process based on horizontal circulating tube type reactor |
| CN112624163A (en) * | 2020-12-01 | 2021-04-09 | 沈阳化工大学 | Magnesium hydroxide production process based on loop reactor |
| CN114956133A (en) * | 2022-05-27 | 2022-08-30 | 华东理工大学 | Method for preparing magnesium hydroxide by extracting potassium, old bittern, magnesium chloride and ammonia gas |
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| CN1467020A (en) * | 2002-07-10 | 2004-01-14 | 北京化工大学精细化工厂 | Method for preparing inorganic nonmetallic nanometer material using static mixer |
| CN101224901A (en) * | 2008-01-30 | 2008-07-23 | 大连海事大学 | Continuous preparation method of high-purity magnesium hydroxide |
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2017
- 2017-08-28 CN CN201710752426.6A patent/CN107572565A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1467020A (en) * | 2002-07-10 | 2004-01-14 | 北京化工大学精细化工厂 | Method for preparing inorganic nonmetallic nanometer material using static mixer |
| CN101224901A (en) * | 2008-01-30 | 2008-07-23 | 大连海事大学 | Continuous preparation method of high-purity magnesium hydroxide |
Non-Patent Citations (1)
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110092408A (en) * | 2019-05-12 | 2019-08-06 | 广东工业大学 | A kind of method of continuous production copper oxide |
| CN112320827A (en) * | 2020-10-10 | 2021-02-05 | 沈阳化工大学 | Process for preparing magnesium hydroxide by cyclic reaction |
| CN112537787A (en) * | 2020-12-01 | 2021-03-23 | 沈阳化工大学 | Magnesium hydroxide continuous production process based on horizontal circulating tube type reactor |
| CN112624163A (en) * | 2020-12-01 | 2021-04-09 | 沈阳化工大学 | Magnesium hydroxide production process based on loop reactor |
| CN114956133A (en) * | 2022-05-27 | 2022-08-30 | 华东理工大学 | Method for preparing magnesium hydroxide by extracting potassium, old bittern, magnesium chloride and ammonia gas |
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Application publication date: 20180112 |