CN110510645A - A kind of method and system cleaning loop production magnesium hydroxide - Google Patents
A kind of method and system cleaning loop production magnesium hydroxide Download PDFInfo
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- CN110510645A CN110510645A CN201910927019.3A CN201910927019A CN110510645A CN 110510645 A CN110510645 A CN 110510645A CN 201910927019 A CN201910927019 A CN 201910927019A CN 110510645 A CN110510645 A CN 110510645A
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- sodium chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The present invention provides a kind of method and system for cleaning loop production magnesium hydroxide, the method includes, chlor-alkali production step S1: saturated sodium chloride solution enters electrolysis unit and is electrolysed, and generates sodium hydroxide solution, chlorine, hydrogen and unsaturated sodium chloride solution；Salting-out step S2: magnesium chloride hexahydrate crystal and the unsaturated sodium chloride solution enter salt analysis apparatus, and precipitated sodium chloride crystal generates magnesium chloride solution；Magnesium hydroxide production stage S3: the magnesium chloride solution and the sodium hydroxide solution enter magnesium hydroxide synthesizer, and reaction generates the first slurry；First slurry enters the first filter press and is filtered washing, generates the first magnesium hydroxide filter cake and the first sodium chloride filtrate；After the first magnesium hydroxide filter cake is dried, magnesium hydroxide products are obtained.According to the technique and scheme of the present invention, by combining chloralkali process with magnesium hydroxide production technology, the circulation comprehensive that can be realized resource is utilized.
Description
Technical field
This patent disclosure relates generally to the comprehensive utilization of resources fields of inorganic chemical product, close more particularly, to a kind of cleaning
Ring produces magnesium hydroxide technology.
Background technique
Magnesium hydroxide is to be only second to magnesia in magnesium chemicals and light calcined magnesia occupies the magnesium chemicals of third position, and close
External magnesia refractories manufacturer adjusts the product mix over year, and in non-fire resistive material field, yield highest, kind are most, answer
It with the most commonly used kind in field, while being also that developed country is pursuing the strategy of sustainable development, protect environment, sending out beneficial to ecology
By one of favor and the product praised highly in exhibition process.Referred to as green safe neutralizer, environmental-friendly fire retardant and the third
Alkali.Therefore, in addition to developed country continues to keep powerful growth momentum, some less developed countries also aim at this product, present
The a piece of situation competitively developed.Production method mainly has 2 kinds, and one is being produced using natural crystal, another kind is chemical synthesis
Method.Its purposes mainly has 4 kinds: (1) in environment protection field, being widely used in neutralizing acid waste water, flue gas desulfurization, processing containing heavy metal
Waste liquid etc.；(2) in flame retardant area, it is used as the inorganic fire retardants of high polymer；(3) in terms of aquaculture, magnesium hydroxide can be made
For alkalescent neutralizer, weaken acidification caused by farm accumulates because of organic matter and be inclined to, and it is thin to can inhibit sulfate reduction
The breeding of bacterium；(4) in other respects, such as oil product vanadium-inhibiting agent, additive, electronic component or coating electronic ceramics field.
Magnesium hydroxide, by more and more extensive concern, is the most hot magnesium compound field of Recent study in inorganic fire retardants field.
Magnesium hydroxide is produced to be greater than and be asked, Market competition.
China's magnesium compound industry raw material is solvable mainly from magnesia nonmetallic ore, brine, Bischofite in Salt lake, magnesium sulfate
Magnesium salts etc..As country renovates the environmental protection of mining and chemical company, most of magnesia nonmetallic ore is closed to prohibit and be adopted, magnesium
Commodities company's industry is closed because lacking raw material and the environmental protection reasons such as not up to standard, face halt production or half is stopped production, such as Hebei silk floss river, Henan monarch ginseng, pellet
Source Dong Jin etc..In order to alleviate magnesium compound production and the energy, resource scarcity, environmental pollution, the contradiction between ecological protection, the world
Various comprehensive utilization of resources production methods efficiently, environmentally friendly, economic are all being studied by each state.With resource-effective, realization environment friend
The Mode of Circular that good and sustainable development is characterized by countries in the world concern and take corresponding behave to increase one after another
The ability of strong sustainable economic development.
Summary of the invention
It is an object of the invention to overcome the waste residue that production magnesium hydroxide generates in the prior art that cannot efficiently use, cause
The defect of environmental pollution and the wasting of resources provides a kind of method and system for cleaning loop production magnesium hydroxide.
According to the first aspect of the invention, a kind of method cleaning loop production magnesium hydroxide is provided, including, chlor-alkali production
Step S1: saturated sodium chloride solution is produced by salt dissolving device；The saturated sodium chloride solution enters electrolysis unit and is electrolysed,
Generate sodium hydroxide solution, chlorine, hydrogen and unsaturated sodium chloride solution；Salting-out step S2: magnesium chloride hexahydrate crystal and institute
It states unsaturated sodium chloride solution and enters salt analysis apparatus, precipitated sodium chloride crystal generates magnesium chloride solution；The sodium chloride crystal returns
It returns the salt dissolving device and carries out salt dissolving, to be deployed into the saturated sodium chloride solution；Magnesium hydroxide production stage S3: the chlorination
Magnesium solution and the sodium hydroxide solution enter magnesium hydroxide synthesizer, and reaction generates the first slurry；First slurry into
Enter the first filter press and be filtered washing, generates the first magnesium hydroxide filter cake and the first sodium chloride filtrate；First sodium chloride
Filtrate returns to the salt dissolving device and carries out salt dissolving, to be deployed into the saturated sodium chloride solution；The first magnesium hydroxide filter cake
After being dried, magnesium hydroxide products are obtained.
Optionally, the magnesium hydroxide production stage S3 further includes that preceding warp is dried in the first magnesium hydroxide filter cake
Cross following steps: the first magnesium hydroxide filter cake enters size-mixing tank and sizes mixing, and generates the second slurry；Second slurry into
Enter the second filter press and carry out pressure filtration washing, obtains the second magnesium hydroxide filter cake, the second sodium chloride filtrate and Washing of Filter Cake water；
The Washing of Filter Cake water returns to the size-mixing tank and sizes mixing to the first magnesium hydroxide filter cake；The second magnesium hydroxide filter
Cake after drying, obtains magnesium hydroxide products.
Optionally, the second sodium chloride filtrate is the solution containing residual magnesium ion, magnesium hydroxide and sodium chloride, described
Method further includes water reuse (treatment processing step S4: the pH value for adjusting the second sodium chloride filtrate is 10~11, so that described second
Magnesium ion in sodium chloride filtrate forms precipitating；It intercepts and separates magnesium hydroxide in the second sodium chloride filtrate and described heavy
It forms sediment, obtains sodium chloride clear solution；The sodium chloride clear solution separates sodium chloride by reverse osmosis, obtains pure water；It is described
Pure water enters at least one of first filter press, second filter press, as slurry.
Optionally, the first sodium chloride filtrate is the sodium chloride solution containing residual magnesium ion, magnesium hydroxide, the side
Method further includes that the first sodium chloride filtrate passes through tail salt treatment step S5: the tail salt treatment before returning to the salt dissolving device
Step S5 includes sequentially adding hydrochloric acid, sodium hydroxide, coagulant, flocculant in Xiang Suoshu the first sodium chloride filtrate, and sink naturally
The supernatant of magnesium hydroxide wadding body and sodium chloride-containing is obtained after drop；The supernatant of the sodium chloride-containing passes through the mistake of fabric filter
Filter, to filter suspended matter, obtains third sodium chloride filtrate；The third sodium chloride filtrate returns to the salt dissolving device
Salt, to be deployed into the saturated sodium chloride solution.
It optionally, further include that the part unsaturated sodium chloride solution enters the salt dissolving device after pervaporation, to adjust
It is made into the saturated sodium chloride solution.
According to the second aspect of the invention, a kind of system cleaning loop production magnesium hydroxide is provided, including, salt dissolving dress
It sets, for producing saturated sodium chloride solution；Electrolysis unit is connected, for receiving the saturated sodium-chloride with the salt dissolving device
Solution is simultaneously electrolysed it, generates sodium hydroxide solution, chlorine, hydrogen and unsaturated sodium chloride solution；Salt analysis apparatus,
It is connected with the electrolysis unit, for receiving the unsaturated sodium chloride solution and it being mixed progress with magnesium chloride hexahydrate crystal
It saltouts, with precipitated sodium chloride crystal and generates magnesium chloride solution；The salt dissolving device, be also used to receive the sodium chloride crystal into
Row salt dissolving, to be deployed into the saturated sodium chloride solution；Magnesium hydroxide synthesizer is filled with the salt analysis apparatus and the electrolysis
It sets connected, for receiving the magnesium chloride solution and the sodium hydroxide solution and reacted, generates the first slurry；First pressure
Filter is connected with the magnesium hydroxide synthesizer and the salt dissolving device, for receiving first slurry and carrying out to it
Filtration washing generates the first magnesium hydroxide filter cake and the first sodium chloride filtrate；The salt dissolving device, is also used to receive described first
Sodium chloride filtrate carries out salt dissolving, to be deployed into the saturated sodium chloride solution；Drier is connected with first filter press, uses
In receiving the first magnesium hydroxide filter cake and it being dried, magnesium hydroxide products are obtained.
It optionally, further include size-mixing tank between first filter press and the drier, with the first filter press phase
Even, for receiving the first magnesium hydroxide filter cake and sizing mixing to it, the second slurry is generated；Second filter press, is connected to
Between the size-mixing tank and the drier, for receiving second slurry and carrying out pressure filtration washing to it, the second hydrogen is obtained
Magnesia filter cake, the second sodium chloride filtrate and Washing of Filter Cake water；The size-mixing tank is also used to receive the Washing of Filter Cake water,
To size mixing to the first magnesium hydroxide filter cake；The drier, for receiving the second magnesium hydroxide filter cake and right
It is dried, and obtains magnesium hydroxide products.
Optionally, the second sodium chloride filtrate is the solution containing residual magnesium ion, magnesium hydroxide and sodium chloride, described
System further includes water reuse (treatment processing unit, is connected with second filter press and first filter press, for receiving described
Dichloride sodium filtrate and to adjust its pH value be 10~11, so that magnesium ion in the second sodium chloride filtrate forms precipitating；Institute
Stating includes ultrafiltration ceramic membrane in water reuse (treatment processing unit, for intercepts separate magnesium hydroxide in the second sodium chloride filtrate with
The precipitating obtains sodium chloride clear solution；Further include reverse osmosis membrane in the water reuse (treatment processing unit, is used for the chlorination
Sodium chloride separation in sodium clear solution, to obtain pure water；And the pure water is returned into first filter press, second pressure
At least one of filter, as slurry.
Optionally, the first sodium chloride filtrate is the sodium chloride solution containing residual magnesium ion, magnesium hydroxide, the system
System further includes that tail salt treatment device is connected between first filter press and the salt dissolving device, for receiving described first
Sodium chloride filtrate simultaneously sequentially adds hydrochloric acid, sodium hydroxide, coagulant, flocculant thereto, and hydroxide is obtained after natural subsidence
The supernatant of magnesium wadding body and sodium chloride-containing；It further include fabric filter in the tail salt treatment device, for the chloride containing
The supernatant of sodium is filtered, and to filter suspended matter, obtains third sodium chloride filtrate；The salt dissolving device, is also used to receive institute
It states third sodium chloride filtrate and carries out salt dissolving, to be deployed into the saturated sodium chloride solution.
Optionally, further include vaporising device, be connected with the electrolysis unit and the salt dissolving device, be used for receiving portion
The unsaturation sodium chloride solution is simultaneously evaporated it, makes it into the salt dissolving device, then to be deployed into the saturation
Sodium chloride solution.
The present invention has the advantages that
1) according to the technique and scheme of the present invention, by combining chloralkali process with magnesium hydroxide production technology, Neng Gou
Meet the comprehensive utilization that resource is realized while chlorine industry and magnesium hydroxide production requirement；
2) according to the technique and scheme of the present invention, the recycling by sodium compound in the entire system realizes sodium money
The cyclic balance in source and effective use realize the clean manufacturing of entire technical process and the zero-emission of waste residue；
3) according to the technique and scheme of the present invention, by water reuse (treatment processing scheme, the recycling of washing water is realized, it is water-saving
Significant effect.
Detailed description of the invention
Fig. 1 shows a kind of system schematic for cleaning loop production magnesium hydroxide according to the present invention.
Fig. 2 shows a kind of a kind of embodiment signals for the system for cleaning loop production magnesium hydroxide according to the present invention
Figure.
Fig. 3 shows a kind of a kind of embodiment signal of system including water reuse (treatment processing unit according to the present invention
Figure.
Fig. 4 shows a kind of a kind of embodiment schematic diagram of system including tail salt treatment device according to the present invention.
Fig. 5 shows a kind of a kind of embodiment schematic diagram of system including vaporising device according to the present invention.
Fig. 6 shows a kind of method flow diagram for cleaning loop production magnesium hydroxide according to the present invention.
Fig. 7 shows the grain size distribution of sodium chloride crystal according to the present invention.
Fig. 8 shows the grain size distribution of magnesium hydroxide products according to the present invention.
Specific embodiment
The preferred embodiments of the present invention will be described in detail with reference to the accompanying drawing, and reference label refers to the group in the present invention
Part, technology, realizing under appropriate circumstances so as to advantages and features of the invention can be easier to be understood.Following description is pair
The materialization of the claims in the present invention, and other specific implementations not clearly stated relevant to claim also belong to power
The range that benefit requires.
Fig. 1 shows a kind of system schematic for cleaning loop production magnesium hydroxide according to the present invention.
As shown in Figure 1, a kind of system for cleaning loop production magnesium hydroxide is provided, including, salt dissolving device 110, for giving birth to
Produce saturated sodium chloride solution；Electrolysis unit 120 is connected, for receiving the saturated sodium chloride solution with the salt dissolving device 110
And it is electrolysed, generate sodium hydroxide solution, chlorine, hydrogen and unsaturated sodium chloride solution；Salt analysis apparatus 130, with
The electrolysis unit 120 is connected, for receiving the unsaturated sodium chloride solution and being mixed into it with magnesium chloride hexahydrate crystal
Row is saltoutd, and with precipitated sodium chloride crystal and generates magnesium chloride solution；The salt dissolving device 110, is also used to receive the sodium chloride
Crystal carries out salt dissolving, to be deployed into the saturated sodium chloride solution；Magnesium hydroxide synthesizer 140, with the salt analysis apparatus 130
It is connected with the electrolysis unit 120, for receiving the magnesium chloride solution and the sodium hydroxide solution and being reacted, generates
The first slurry comprising magnesium hydroxide and sodium chloride；First filter press 150, with the magnesium hydroxide synthesizer 140 and described
Salt dissolving device 110 is connected, for receiving first slurry and be filtered washing to it, generate the first magnesium hydroxide filter cake with
First sodium chloride filtrate；The salt dissolving device 110 is also used to receive the first sodium chloride filtrate and carries out salt dissolving, to be deployed into
The saturated sodium chloride solution；Drier 160 is connected with first filter press 150, for receiving first magnesium hydroxide
Filter cake is simultaneously dried it, obtains magnesium hydroxide products.
The electrolysis unit 120 is electrolysed with saturated sodium chloride solution, can both accelerate reaction rate, also because of chlorine
Meltage in saturated sodium chloride solution is smaller.The saturated sodium chloride solution in the electrolysis unit 120 can pass through
The salt dissolving device 110 provides.The salt dissolving device 110 can be adjusts solid sodium chloride and water according to a certain percentage
Match, is also possible to the solid sodium chloride and unsaturated sodium chloride solution such as deploy, to generate saturated sodium chloride solution.Example
Such as, the salt dissolving device 110 can receive the sodium chloride crystal and first filter press that the salt analysis apparatus 130 generates
150 the first sodium chloride filtrates generated are deployed the circulation comprehensive benefit that sodium resource is realized to produce saturated sodium chloride solution
With.The electrolysis unit 120 can be connected directly or be indirectly connected with the salt dissolving device 110.For example, the salt dissolving dress
The saturated sodium chloride solution produced in 110 is set before being electrolysed into the electrolysis unit 120, can also be carried out as needed
Removal of impurities, to remove the calcium ions and magnesium ions etc. in the saturated sodium chloride solution.
The salt analysis apparatus 130 is greater than the original of the solubility of sodium chloride according to common-ion effect and the solubility of magnesium chloride
Reason, saltouts after mixing unsaturated sodium chloride solution with magnesium chloride hexahydrate crystal, precipitated sodium chloride crystal, magnesium chloride hexahydrate
Crystal is dissolved in water and generates magnesium chloride solution, both can make to separate by the modes such as filtering, being centrifugated.The magnesium chloride solution
The magnesium hydroxide synthesizer 140 can be entered back into after purified treatment.The purified treatment, which can be, utilizes ceramic membrane
Etc. modes intercept the insoluble matter in solution.The magnesium chloride hexahydrate also known as water chlorine stone, halogen piece, halogen powder, chemical formula MgCl2·
6H2O may come from salt lake or produce the by-product of other products, such as by-product when production potash fertilizer.The unsaturation
Sodium chloride solution can be the sodium chloride solution of the 203g/L generated after electrolysis saturated sodium chloride solution.The salt analysis apparatus 130
The unsaturated sodium chloride solution that the electrolysis unit 120 generates is utilized, fully utilizes part water, reduces the unsaturation
The evaporation capacity of water in sodium chloride solution, greatly reduces energy consumption.
First slurry is the magnesium hydroxide and sodium chloride that reaction generates, and may not no fully reacting magnesium chloride
Deng mixed slurry.After the filters pressing and washing of first filter press 150, the first magnesium hydroxide filter cake and the first chlorine are obtained
Change sodium filtrate.It may be also containing residual magnesium ion, magnesium hydroxide in the first sodium chloride filtrate.The first sodium chloride filtrate
It can be all filtrates obtained when first filter press 150 carries out pressure filtration washing to first slurry, including after washing
Filtrate etc..It can be connected directly or be indirectly connected between first filter press 150 and the salt dissolving device 110.Example
Such as, the first sodium chloride filtrate can directly return to the salt dissolving device 110 and carry out salt dissolving processing, can also by removal of impurities with
The salt dissolving device 110 is returned again to after removing residual magnesium ion and magnesium hydroxide.Removal of impurities can according to need or residual impurity
Amount chooses whether to carry out or carry out in which step.For example, the first sodium chloride filtrate directly returns to the salt dissolving device
110, if impurity content is more can also to clean after salt dissolving, enters back into electrolysis unit 120 and participate in cell reaction.It is described
First filter press 150 can be horizontal pressure filter etc..
The drier 160 is directly or indirectly connected with first filter press 150.The first magnesium hydroxide filter cake
It can convey, can also be conveyed through feeding spiral conveyer through belt feeder, to be transported to the drier 160.The drier
160 can be flash distillation dryer etc..Drying source can use natural gas.The magnesium hydroxide products obtained after drying can be with
It is packed into automatic packaging machine.After magnesium hydrate powder after drying may also pass through calcining furnace calcining, to be aoxidized
Magnesium products.Therefore, it can be also used for production magnesium oxide product according to the technique and scheme of the present invention.The high temperature tail that calcination process generates
Gas can return to the drier 160, to use as dry heat source, can be realized the recycling of the energy, in this way to reach
To the purpose of energy-saving and emission-reduction.
It according to the technique and scheme of the present invention, can be full by combining chloralkali process with magnesium hydroxide production technology
The comprehensive utilization of resource is realized while sufficient chlorine industry and magnesium hydroxide production requirement.In the entire system by sodium compound
Recycling, cyclic balance and the effective use of sodium resource may be implemented.In this cyclic process, sodium be it is nonexpendable,
Therefore it in addition to normal loss may need additionally to add sodium chloride into the salt dissolving device 110, does not need to add chlorination again
Sodium or sodium hydroxide.And other than product magnesium hydroxide or magnesia generate, also generated without additional waste residue, thus
Realize the clean manufacturing of entire technical process and the zero-emission of waste residue.
Fig. 2 shows a kind of a kind of embodiment signals for the system for cleaning loop production magnesium hydroxide according to the present invention
Figure.
As shown in Fig. 2, can also include size-mixing tank 210 between first filter press 150 and the drier 160, with
First filter press 150 is connected, and for receiving the first magnesium hydroxide filter cake and sizing mixing to it, generates the second slurry
Material；Second filter press 220 is connected between the size-mixing tank 210 and the drier 160, for receiving second slurry
And pressure filtration washing is carried out to it, obtain the second magnesium hydroxide filter cake, the second sodium chloride filtrate and Washing of Filter Cake water；The tune
Stock tank 210 is also used to receive the Washing of Filter Cake water, to size mixing to the first magnesium hydroxide filter cake；The drier
160, for receiving the second magnesium hydroxide filter cake and it being dried, obtain magnesium hydroxide products.
The size-mixing tank 210 can be used for that the first magnesium hydroxide filter cake is sized mixing and washed, and pass through second
The filters pressing and washing of filter press 220, to achieve the purpose that further cleaning to the first magnesium hydroxide filter cake, with further
Improve the purity of magnesium hydroxide products.According to the present embodiment, the purity for the magnesium hydroxide products produced can achieve 99%
More than.Second filter press 220 can be vertical type blotter press etc..Second filter press 220 carries out second slurry
The process of pressure filtration washing can be, when filters pressing generates filter cake and the second sodium chloride filtrate, then washs to filter cake, available
Washing of Filter Cake water.The Washing of Filter Cake water returns to the size-mixing tank 210 as the mother liquor or plasm scouring water uses again of sizing mixing, can be with
Washing water is effectively recycled, water resource is saved.
Fig. 3 shows a kind of a kind of embodiment signal of system including water reuse (treatment processing unit according to the present invention
Figure.
As shown in figure 3, the second sodium chloride filtrate is the solution containing residual magnesium ion, magnesium hydroxide and sodium chloride,
The system can also include water reuse (treatment processing unit 310, with second filter press 220 and 150 phase of the first filter press
It even, is 10~11 for receiving the second sodium chloride filtrate and adjusting its pH value, so that in the second sodium chloride filtrate
Magnesium ion forms precipitating；Include ultrafiltration ceramic membrane in the water reuse (treatment processing unit 310, separates second chlorination for intercepting
Magnesium hydroxide and the precipitating in sodium filtrate, obtain sodium chloride clear solution；Further include in the water reuse (treatment processing unit 310
Reverse osmosis membrane, for separating the sodium chloride in the sodium chloride clear solution, to obtain pure water；And the pure water is returned into institute
At least one of the first filter press 150, described second filter press 220 are stated, as slurry.
The second sodium chloride filtrate is due to being to carry out filters pressing generation to second slurry, wherein containing a small amount of
Magnesium ion, magnesium hydroxide and sodium chloride.It is 10~11 that the solution, which is adjusted pH value, such as when 10.5, magnesium ion forms precipitating effect
Fruit is obvious, especially effectively can all precipitate the magnesium ion in the second sodium chloride filtrate when pH value is 10.5.
The magnesium hydrate precipitate that the magnesium hydroxide of script and adjusting pH value are formed later in the second sodium chloride filtrate can pass through
Ultrafiltration ceramic membrane intercepts separation, and can be with recycling and reusing, such as forms product after treatment.The reverse osmosis membrane separation institute
It states the sodium chloride that sodium chloride clear solution obtains and can be recycled to the salt dissolving device 110 and utilized again.The pure water is
Salt content is less than the water of 30ppm, can be used as slurry recycling.According to the present embodiment, following for washing water is realized
Ring uses, and water-saving result is significant.
Fig. 4 shows a kind of a kind of embodiment schematic diagram of system including tail salt treatment device according to the present invention.
As shown in figure 4, the first sodium chloride filtrate is the sodium chloride solution containing residual magnesium ion, magnesium hydroxide, institute
The system of stating can also include tail salt treatment device 410, be connected to first filter press 150 and the salt dissolving device 110 it
Between, for receiving the first sodium chloride filtrate and sequentially adding hydrochloric acid, sodium hydroxide, coagulant, flocculant thereto, to certainly
So the supernatant of magnesium hydroxide wadding body and sodium chloride-containing is obtained after sedimentation；It further include fiber mistake in the tail salt treatment device 410
Filter is filtered for the supernatant to the sodium chloride-containing, to filter suspended matter, obtains third sodium chloride filtrate；It is described
Salt dissolving device 110 is also used to receive the third sodium chloride filtrate and carries out salt dissolving, to be deployed into the saturated sodium chloride solution.
The tail salt treatment device 410 in present embodiment is one to clean to the first sodium chloride filtrate
For example, system of the invention can be not limited to this removal of impurities mode in the case where there is removal of impurities to need.First chlorination
Sodium filtrate is due to being the solution reacted in magnesium hydroxide synthesizer 140, and sodium chloride is major solute, wherein may
It has remaining magnesium ion and wears the magnesium hydroxide etc. of filter.The first sodium chloride filtrate can be collected by collecting tank, then defeated
It send to the tail salt treatment device 410.By the way that hydrochloric acid is added into the first sodium chloride filtrate, make the magnesium hydroxide in solution
All dissolutions, it is unfavorable to remove ultra-small grain size magnesium hydroxide crystal that may be present, ultra-small grain size magnesium hydroxide crystal in solution
In later separation；Add sodium hydroxide, the magnesium ion in solution can be made to be completely formed precipitating, and by be added coagulant and
Flocculant has the magnesium hydrate precipitate to be formed to facilitate separation in the form of wadding body, is separated after natural subsidence, institute
The supernatant of sodium chloride-containing is stated by the suspended matter in the fabric filter again filtering solution, after processing qualified chlorination
Sodium solution is the third sodium chloride filtrate.The third sodium chloride filtrate returns to the salt dissolving device 110 and carries out salt dissolving, real
The circulation comprehensive for having showed resource utilizes.
Fig. 5 shows a kind of a kind of embodiment schematic diagram of system including vaporising device according to the present invention.
As shown in figure 5, can also include vaporising device 510, with the electrolysis unit 120 and 110 phase of salt dissolving device
Even, for unsaturation sodium chloride solution described in receiving portion and it is evaporated, then makes it into the salt dissolving device
110, to be deployed into the saturated sodium chloride solution.
The unsaturation sodium chloride solution can fully enter the salt analysis apparatus 130 and saltout, can also be according to life
It produces and part is needed to enter the evaporation that the vaporising device 510 carries out excessive moisture, then enter back into the salt dissolving device 110 and carry out
Salt dissolving.For example, if the unsaturation sodium chloride solution according to production needs, cannot or not need to fully enter described saltout
Device 130 is saltoutd, then the extra part unsaturated sodium chloride solution can be evaporated and recycle, so that its
It can recycle in system and utilize again, avoid the wasting of resources and the generation of waste residue.
Fig. 6 shows a kind of method flow diagram for cleaning loop production magnesium hydroxide according to the present invention.
As shown in fig. 6, a kind of method for cleaning loop production magnesium hydroxide is provided, including, chlor-alkali production step S1: pass through
Salt dissolving device produces saturated sodium chloride solution；The saturated sodium chloride solution enters electrolysis unit and is electrolysed, and generates hydroxide
Sodium solution, chlorine, hydrogen and unsaturated sodium chloride solution；Salting-out step S2: magnesium chloride hexahydrate crystal and the unsaturated chlorine
Change sodium solution and enter salt analysis apparatus, precipitated sodium chloride crystal generates magnesium chloride solution；The sodium chloride crystal returns to the salt dissolving
Device carries out salt dissolving, to be deployed into the saturated sodium chloride solution；Magnesium hydroxide production stage S3: the magnesium chloride solution and institute
It states sodium hydroxide solution and enters magnesium hydroxide synthesizer, reaction generates the first slurry；First slurry enters the first filters pressing
Machine is filtered washing, generates the first magnesium hydroxide filter cake and the first sodium chloride filtrate；The first sodium chloride filtrate returns to institute
It states salt dissolving device and carries out salt dissolving, to be deployed into the saturated sodium chloride solution；After the first magnesium hydroxide filter cake is dried,
Obtain magnesium hydroxide products.
A kind of embodiment according to the present invention, the magnesium hydroxide production stage S3 further include first hydroxide
Magnesium filter cake passes through following steps before being dried: the first magnesium hydroxide filter cake enters size-mixing tank and sizes mixing, and generates second
Slurry；Second slurry enters the second filter press and carries out pressure filtration washing, obtains the second magnesium hydroxide filter cake, the filter of the second sodium chloride
Liquid and Washing of Filter Cake water；The Washing of Filter Cake water returns to the size-mixing tank and sizes mixing to the first magnesium hydroxide filter cake；
The second magnesium hydroxide filter cake after drying, obtains magnesium hydroxide products.
A kind of embodiment according to the present invention, the second sodium chloride filtrate are containing residual magnesium ion, magnesium hydroxide
With the solution of sodium chloride, the method also includes water reuse (treatment processing step S4: the pH value for adjusting the second sodium chloride filtrate is
10~11, so that the magnesium ion in the second sodium chloride filtrate forms precipitating；It intercepts and separates in the second sodium chloride filtrate
Magnesium hydroxide and the precipitating, obtain sodium chloride clear solution；The sodium chloride clear solution is by reverse osmosis by sodium chloride
Separation, obtains pure water；The pure water enters at least one of first filter press, second filter press, as washing
Use water.
A kind of embodiment according to the present invention, the first sodium chloride filtrate are containing residual magnesium ion, magnesium hydroxide
Sodium chloride solution, the method also includes the first sodium chloride filtrate passes through tail salt treatment before returning to the salt dissolving device
Step S5: the tail salt treatment step S5 includes sequentially adding hydrochloric acid in Xiang Suoshu the first sodium chloride filtrate, sodium hydroxide, mixing
Solidifying agent, flocculant, and the supernatant of magnesium hydroxide wadding body and sodium chloride-containing is obtained after natural subsidence；The supernatant of the sodium chloride-containing
Liquid obtains third sodium chloride filtrate by the filtering of fabric filter to filter suspended matter；The third sodium chloride filtrate returns
The salt dissolving device carries out salt dissolving, to be deployed into the saturated sodium chloride solution.
A kind of embodiment according to the present invention further includes that the part unsaturated sodium chloride solution is laggard through pervaporation
Enter the salt dissolving device, to be deployed into the saturated sodium chloride solution.
Method of the invention hereinbefore has been combined system and is described in detail and explains, will no longer go to live in the household of one's in-laws on getting married here
It states.
Fig. 7 shows the grain size distribution of sodium chloride crystal according to the present invention.Wherein, (a) in Fig. 7 shows chlorination
The grading curve figure of sodium crystal；(b) in Fig. 7 shows the transmission electron microscope picture of sodium chloride crystal.
As shown in fig. 7, according to the technique and scheme of the present invention, the sodium chloride saltoutd in the salt analysis apparatus 130
Crystal particle diameter is evenly distributed, and can satisfy electrolysis and requires.
Fig. 8 shows the grain size distribution of magnesium hydroxide products according to the present invention.Wherein, (a) in Fig. 8 shows hydrogen
The grading curve figure of magnesium oxide product；(b) in Fig. 8 shows the transmission electron microscope picture of magnesium hydroxide products.
As shown in figure 8, according to the technique and scheme of the present invention, the particle diameter distribution of the magnesium hydroxide products of preparation is uniform, product
It is high-quality；And granularity is averagely about 50 μm, granularity can significantly reduce greatly filtering and energy consumption for drying.
Advantages of the present invention at least that:
1) according to the technique and scheme of the present invention, by combining chloralkali process with magnesium hydroxide production technology, Neng Gou
Meet the comprehensive utilization that resource is realized while chlorine industry and magnesium hydroxide production requirement；
2) according to the technique and scheme of the present invention, the recycling by sodium compound in the entire system realizes sodium money
The cyclic balance in source and effective use realize the clean manufacturing of entire technical process and the zero-emission of waste residue；And it forms
The cleaning loop production mode of " resource-production-product-consumption-waste renewable resources-production-product-consumption "；
3) according to the technique and scheme of the present invention, by water reuse (treatment processing scheme, the recycling of washing water is realized, it is water-saving
Significant effect.
It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and this
Field technical staff can be designed alternative embodiment without departing from the scope of the appended claims.In claim
In, any reference symbol between parentheses should not be configured to limitations on claims.
Claims (10)
1. a kind of method for cleaning loop production magnesium hydroxide, including,
Chlor-alkali production step (S1):
Saturated sodium chloride solution is produced by salt dissolving device；
The saturated sodium chloride solution enters electrolysis unit and is electrolysed, and generates sodium hydroxide solution, chlorine, hydrogen and not
Saturated sodium chloride solution；
Salting-out step (S2):
Magnesium chloride hexahydrate crystal and the unsaturated sodium chloride solution enter salt analysis apparatus, and precipitated sodium chloride crystal generates chlorination
Magnesium solution；
The sodium chloride crystal returns to the salt dissolving device and carries out salt dissolving, to be deployed into the saturated sodium chloride solution；
Magnesium hydroxide production stage (S3):
The magnesium chloride solution and the sodium hydroxide solution enter magnesium hydroxide synthesizer, and reaction generates the first slurry；
First slurry enters the first filter press and is filtered washing, generates the first magnesium hydroxide filter cake and the filter of the first sodium chloride
Liquid；
The first sodium chloride filtrate returns to the salt dissolving device and carries out salt dissolving, to be deployed into the saturated sodium chloride solution；
After the first magnesium hydroxide filter cake is dried, magnesium hydroxide products are obtained.
2. according to the method described in claim 1, the magnesium hydroxide production stage (S3) further includes, first magnesium hydroxide
Filter cake passes through following steps before being dried:
The first magnesium hydroxide filter cake enters size-mixing tank and sizes mixing, and generates the second slurry；
Second slurry enters the second filter press and carries out pressure filtration washing, obtains the second magnesium hydroxide filter cake, the filter of the second sodium chloride
Liquid and Washing of Filter Cake water；
The Washing of Filter Cake water returns to the size-mixing tank and sizes mixing to the first magnesium hydroxide filter cake；
The second magnesium hydroxide filter cake after drying, obtains magnesium hydroxide products.
3. according to the method described in claim 2, wherein, the second sodium chloride filtrate is containing residual magnesium ion, hydroxide
The solution of magnesium and sodium chloride, the method also includes,
Water reuse (treatment processing step (S4):
The pH value for adjusting the second sodium chloride filtrate is 10~11, so that the magnesium ion in the second sodium chloride filtrate is formed
Precipitating；
Magnesium hydroxide and the precipitating separated in the second sodium chloride filtrate is intercepted, sodium chloride clear solution is obtained；
The sodium chloride clear solution separates sodium chloride by reverse osmosis, obtains pure water；
The pure water enters at least one of first filter press, second filter press, as slurry.
4. according to the method described in claim 1, wherein, the first sodium chloride filtrate is containing residual magnesium ion, hydroxide
The sodium chloride solution of magnesium, the method also includes the first sodium chloride filtrate is passed through at tail salt before returning to the salt dissolving device
It manages step (S5):
The tail salt treatment step (S5) includes,
Hydrochloric acid, sodium hydroxide, coagulant, flocculant are sequentially added into the first sodium chloride filtrate, and after natural subsidence
To the supernatant of magnesium hydroxide wadding body and sodium chloride-containing；
The supernatant of the sodium chloride-containing obtains third sodium chloride filtrate by the filtering of fabric filter to filter suspended matter；
The third sodium chloride filtrate returns to the salt dissolving device and carries out salt dissolving, to be deployed into the saturated sodium chloride solution.
5. according to the method described in claim 1, further include,
The part unsaturated sodium chloride solution enters the salt dissolving device after pervaporation, to be deployed into the saturated sodium-chloride
Solution.
6. a kind of system for cleaning loop production magnesium hydroxide, including,
Salt dissolving device, for producing saturated sodium chloride solution；
Electrolysis unit is connected with the salt dissolving device, for receiving the saturated sodium chloride solution and being electrolysed to it, generates
Sodium hydroxide solution, chlorine, hydrogen and unsaturated sodium chloride solution；
Salt analysis apparatus is connected with the electrolysis unit, for receiving the unsaturated sodium chloride solution and by itself and six water chlorinations
Magnesium crystal mixing is saltoutd, and with precipitated sodium chloride crystal and generates magnesium chloride solution；
The salt dissolving device is also used to receive the sodium chloride crystal and carries out salt dissolving, to be deployed into the saturated sodium chloride solution；
Magnesium hydroxide synthesizer is connected, for receiving the magnesium chloride solution with the salt analysis apparatus and the electrolysis unit
With the sodium hydroxide solution and reacted, generate the first slurry；
First filter press is connected with the magnesium hydroxide synthesizer and the salt dissolving device, for receiving first slurry
And washing is filtered to it, generate the first magnesium hydroxide filter cake and the first sodium chloride filtrate；
The salt dissolving device is also used to receive the first sodium chloride filtrate and carries out salt dissolving, to be deployed into the saturated sodium-chloride
Solution；
Drier is connected with first filter press, for receiving the first magnesium hydroxide filter cake and it being dried, obtains
To magnesium hydroxide products.
7. system according to claim 6 further includes between first filter press and the drier,
Size-mixing tank is connected with first filter press, raw for receiving the first magnesium hydroxide filter cake and sizing mixing to it
At the second slurry；
Second filter press is connected between the size-mixing tank and the drier, for receive second slurry and to its into
Row pressure filtration washing obtains the second magnesium hydroxide filter cake, the second sodium chloride filtrate and Washing of Filter Cake water；
The size-mixing tank is also used to receive the Washing of Filter Cake water, to size mixing to the first magnesium hydroxide filter cake；
The drier obtains magnesium hydroxide products for receiving the second magnesium hydroxide filter cake and it being dried.
8. system according to claim 7, wherein the second sodium chloride filtrate is containing residual magnesium ion, hydroxide
The solution of magnesium and sodium chloride, the system also includes,
Water reuse (treatment processing unit is connected with second filter press and first filter press, for receiving second chlorination
Sodium filtrate and to adjust its pH value be 10~11, so that magnesium ion in the second sodium chloride filtrate forms precipitating；
It include ultrafiltration ceramic membrane in the water reuse (treatment processing unit, for intercepting the hydrogen-oxygen separated in the second sodium chloride filtrate
Change magnesium and the precipitating, obtains sodium chloride clear solution；
It further include reverse osmosis membrane in the water reuse (treatment processing unit, for dividing the sodium chloride in the sodium chloride clear solution
From to obtain pure water；And the pure water is returned at least one of first filter press, described second filter press, as
Slurry.
9. system according to claim 6, wherein the first sodium chloride filtrate is containing residual magnesium ion, hydroxide
The sodium chloride solution of magnesium, the system also includes,
Tail salt treatment device is connected between first filter press and the salt dissolving device, for receiving first chlorination
Sodium filtrate simultaneously sequentially adds hydrochloric acid, sodium hydroxide, coagulant, flocculant thereto, and magnesium hydroxide wadding is obtained after natural subsidence
The supernatant of body and sodium chloride-containing；
Further include fabric filter in the tail salt treatment device, is filtered for the supernatant to the sodium chloride-containing, with
Suspended matter is filtered, third sodium chloride filtrate is obtained；
The salt dissolving device is also used to receive the third sodium chloride filtrate and carries out salt dissolving, to be deployed into the saturated sodium-chloride
Solution.
10. according to the method described in claim 6, further include,
Vaporising device is connected with the electrolysis unit and the salt dissolving device, molten for unsaturation sodium chloride described in receiving portion
Liquid is simultaneously evaporated it, then makes it into the salt dissolving device, to be deployed into the saturated sodium chloride solution.
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