CN108622923A - The method of alumina purifying - Google Patents
The method of alumina purifying Download PDFInfo
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- CN108622923A CN108622923A CN201810322688.3A CN201810322688A CN108622923A CN 108622923 A CN108622923 A CN 108622923A CN 201810322688 A CN201810322688 A CN 201810322688A CN 108622923 A CN108622923 A CN 108622923A
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- crystallizer
- melting
- crystal layer
- solution
- alumina
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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
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/46—Purification of aluminium oxide, aluminium hydroxide or aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses the production technologies for the aluminium oxide that high-purity is prepared using fusion-crystallization comprising following steps：First chilled brine is passed through in melting crystallizer external jacket bottom, chilled brine is in uniformly film evaporation device in crystallizer outer wall, then thick alumina solution is put into melting crystallizer, alumina solution is under crystallizer inner wall falling liquid film stream, it gradually cools down and crystallizes, uniform crystal layer is gradually grown on heat-transfer surface, the concentration of crystal layer is higher than the concentration of mixture solution, and impurity is gradually enriched in mixture solution；Then hot water temperature is adjusted by heat exchanger and part melt operation is carried out to crystal layer, so that the low-melting impurities part being mingled in crystal layer fusing is excluded, further to purify crystal.The method and process of the present invention is simple, and device structure is compact, using falling liquid film form, reduces energy, while reducing cost and equipment investment；The product purity produced using the melting crystallizer is high.
Description
Technical field
The present invention relates to the methods of purification of aluminium oxide, the especially method of melting crystallizer alumina purifying.
Background technology
Aluminium oxide and its sylvite can inhibit fungus growth, are used as food preservative for a long time, especially in low ph value, can make
Antisepsis is played for non-dissociated acid.Aluminium oxide has the characteristics that other preservatives are unexistent, that is, has very strong anti-corrosion selectivity,
It can inhibit the growth to human hazard bacterium, and then harmless to the bacterium for being beneficial to people, such as it can inhibit fill cheese moulds life
Growth that is long but having no effect on the bacterium for helping cheese curing.Therefore aluminium oxide is largely used as cheese, cake in the food industry
With the preservative of other cakes.It is mainly used for cheese, pickless, dry fruit, fruit juice, fruit sugar syrups, beverage, preserved fruit, face
Packet, candy etc. it is mould proof.It is also used for the fresh-keeping of flesh of fish product.It is also applied to cosmetics, medicine, feed etc..At present both at home and abroad
The equipment of large-scale production aluminium oxide is general enamel reaction still, the process of maturation process approximately as：Take ketenes
Under the effect of the catalyst with crotonaldehyde, condensation reaction occurs, then the processes acquisition finished product such as hydrolyzes, dry, pack, however due to
The aluminium oxide appearance that the technique productions go out is very secondary, and impurity is more, irritant smell.Therefore it the technique of existing this aluminium oxide and sets
It has to be modified.
Invention content
The technical problem to be solved in the present invention is to provide the methods of melting crystallizer alumina purifying, with good flat
Row reaction selectivity and safety, reduce cost and equipment investment；It is environmentally friendly, less energy consumption, and alumina product purity
High, stay in grade.
In order to solve the above technical problems, the technical solution adopted by the present invention is：The method of alumina purifying, innovative point exist
In：Using melting crystallizer alumina purifying, the specific steps are：
(1) it crystallizes：It is passed through chilled brine in melting crystallizer external jacket bottom, chilled brine is uniformly in melting crystallizer
Outer wall is in film evaporation device, thick alumina solution is put into melting crystallizer, thick alumina solution is in melting crystallizer inner wall
Falling liquid film flows down, and gradually cools down and crystallizes, and uniform crystal layer is gradually grown on heat-transfer surface, the concentration of crystal layer is higher than melting
The concentration of solution, impurity are gradually enriched in solution in crystallizer；
(2) sweating, fusing：After chilled brine is passed through 30~40min, stops feed, hot water is then adjusted by heat exchanger
Temperature carries out part fusing to crystal layer, so that the low-melting impurities being mingled in crystal layer fusing is excluded, further purifies crystal.
The present invention realizes substance separation and purification using melting crystallizer using the difference of solidification point between separate substance,
Transmission by adjusting energy controls mass transfer, to achieve the effect that improve the purity of crystalline rate and crystal product；It improves
Parallel reaction selectivity；For using the recrystallization of solvent the systems of insecurity such as can set off an explosion, burn, pass through melting
Crystallizer control input, maintains the optium concentration of crystallization, low-temperature operation that security of system can be improved；In crystallizer upper airway
It is passed through suitable compressed air, so that solution is formed the rising of slug flow bubble in crystallizer, causes the turbulence of melt, mass transfer enhancement
And heat transfer property.
Further, the crystallisation step is specially：First chilled brine, temperature are passed through in melting crystallizer external jacket bottom
It it is -10 DEG C~-2 DEG C, chilled brine is in uniformly film evaporation device in melting crystallizer outer wall, then puts into thick alumina solution
Into melting crystallizer, while by melting crystallizer gas-guide tube with 4~7m3The speed of/min is passed through into thick alumina solution
Compressed air is allowed to form the rising of slug flow bubble in crystallizer, causes the turbulence of melt, mass transfer enhancement and heat transfer property,
Alumina solution is gradually cooled down and is crystallized under melting crystallizer inner wall falling liquid film stream, is gradually grown on heat-transfer surface uniform
Crystal layer, the concentration of crystal layer are higher than the concentration of solution in melting crystallizer, and impurity is gradually enriched in solution.
Further, the sweating, fusing step are specially：After control chilled brine is passed through 30~40min of time, stop
Feed, switching warm water tank carry out part fusing to crystal layer, and water temperature is 88~92 DEG C, and warm water is passed through the time as 15~40min；So
Switching hot-water cylinder water temperature, which is 90~94 DEG C, afterwards makes the low-melting impurities being mingled in crystal layer fusing exclude, and further purifies crystal,
Hot water is passed through the time as 25~35min.
Further, the chilled brine is calcium chloride solution or sodium chloride solution.
Further, the melting crystallizer is the falling film melt crystallization device of vertical array tubular heat exchanger type.
Compared with the prior art, the advantages of the present invention are as follows：Pass through the technique letter of above-mentioned melting crystallizer alumina purifying
It is single, with good parallel reaction selectivity and safety, using falling liquid film form and low-temperature operation, the energy of specific yield product
Amount consumption is greatly lowered, and has preferable economy, while the technical process crystal is to form crystal layer in heating surface, without
It is suspended in liquid, this avoid the blockings of equipment and pipeline, reduce the generation of fault in production, reduce cost and set
Standby investment；It is environmentally friendly almost without " three wastes " in production process, compared with the recrystallization for using solvent, do not need drying
To remove solvent, energy consumption is only the 10%~30% of rectifying, and the alumina product purity produced using the melting crystallizer
High, stay in grade, increasing operation series can be such that purity infinitely improves, and impurity content can be made in product from percentage composition to ppm
Content, to overcome deficiency in the prior art.
Specific implementation mode
It elaborates to technical scheme of the present invention with reference to specific embodiment.
Embodiment 1
The technique of melting crystallizer alumina purifying, includes the following steps：
(1) it crystallizes：It first is passed through -8 DEG C of calcium chloride solution in melting crystallizer external jacket bottom, calcium chloride solution is uniform
It is in film evaporation device in melting crystallizer outer wall, then puts into the alumina solution being condensed in melting crystallizer, leads to simultaneously
Melting crystallizer gas-guide tube is crossed using compressor with 4m3The compressed air that the speed of/min is passed through into alumina solution, is allowed to
Slug flow bubble is formed in crystallizer to rise, and the turbulence of melt, mass transfer enhancement and heat transfer property, alumina solution is caused to tie
Brilliant device inner wall falling liquid film flows down, and gradually cools down and crystallizes, uniform crystal layer, the concentration of crystal layer are gradually grown on heat-transfer surface
Higher than the concentration of solution in melting crystallizer, impurity is gradually enriched in solution；
(2) sweating, fusing：After control calcium chloride solution is passed through time 30min, stop feed, switching warm water tank is to crystal
Layer carries out part fusing, and warm water tank water temperature is 88 DEG C, and warm water is passed through the time as 15min；Then switching hot-water cylinder makes in crystal layer
The low-melting impurities fusing being mingled with excludes, and further purifies crystal, and hot-water cylinder water temperature is 88 DEG C, and it is 28min that hot water, which is passed through the time,
The purity for obtaining aluminium oxide is 99.91%.
Embodiment 2
The technique of melting crystallizer alumina purifying, includes the following steps：
(1) it crystallizes：It first is passed through -6 DEG C of sodium chloride solution in melting crystallizer external jacket bottom, sodium chloride solution is uniform
It is in film evaporation device in melting crystallizer outer wall, then puts into the alumina solution being condensed in melting crystallizer, leads to simultaneously
Melting crystallizer gas-guide tube is crossed using compressor with 5m3The compressed air that the speed of/min is passed through into alumina solution, is allowed to
Slug flow bubble is formed in crystallizer to rise, and the turbulence of melt, mass transfer enhancement and heat transfer property, alumina solution is caused to tie
Brilliant device inner wall falling liquid film flows down, and gradually cools down and crystallizes, uniform crystal layer, the concentration of crystal layer are gradually grown on heat-transfer surface
Higher than the concentration of solution in melting crystallizer, impurity is gradually enriched in solution；
(2) sweating, fusing：After control sodium chloride solution is passed through time 35min, stop feed, switching warm water tank is to crystal
Layer carries out part fusing, and warm water tank water temperature is 90 DEG C, and warm water is passed through the time as 30min；Then switching hot-water cylinder makes in crystal layer
The low-melting impurities fusing being mingled with excludes, and further purifies crystal, and hot-water cylinder water temperature is 92 DEG C, and it is 30min that hot water, which is passed through the time,
The purity for obtaining aluminium oxide is 99.92%.
Embodiment 3
The technique of melting crystallizer alumina purifying, includes the following steps：
(1) it crystallizes：It first is passed through -2 DEG C of calcium chloride solution in melting crystallizer external jacket bottom, calcium chloride solution is uniform
It is in film evaporation device in melting crystallizer outer wall, then puts into the alumina solution being condensed in melting crystallizer, leads to simultaneously
Melting crystallizer gas-guide tube is crossed using compressor with 7m3The compressed air that the speed of/min is passed through into alumina solution, is allowed to
Slug flow bubble is formed in crystallizer to rise, and the turbulence of melt, mass transfer enhancement and heat transfer property, alumina solution is caused to tie
Brilliant device inner wall falling liquid film flows down, and gradually cools down and crystallizes, uniform crystal layer, the concentration of crystal layer are gradually grown on heat-transfer surface
Higher than the concentration of solution in melting crystallizer, impurity is gradually enriched in solution；
(2) sweating, fusing：After control calcium chloride solution is passed through time 40min, stop feed, switching warm water tank is to crystal
Layer carries out part fusing, and warm water tank water temperature is 92 DEG C, and warm water is passed through the time as 40min；Then switching hot-water cylinder makes in crystal layer
The low-melting impurities fusing being mingled with excludes, and further purifies crystal, and hot-water cylinder water temperature is 94 DEG C, and it is 32min that hot water, which is passed through the time,
The purity for obtaining aluminium oxide is 99.91%.
After the falling film melt crystallization device similar to vertical array tubular heat exchanger, the crystallization process of aluminium oxide becomes more
It is easy to control, impurity is few, and the purity of finished product is higher, generally can reach 99.8% or more, and appearance is whiter and bright, and crystal is good.Pass through
The improvement of the technique does not have or greatly reduces the presence of impurity in aluminium oxide finished product, effectively raises its antiseptic property,
The dosage for reducing preservative in food, effectively raises food security.
Comparative example 1
(1) alumina solution being condensed is got in crystallization kettle, it is cold to lead to cooling water (20~25 DEG C) toward crystallization kettle chuck
When but to 50~60 DEG C, then pre-cooling cycle valve is closed, stops cooling, the aluminium oxide calomel mercurous chloride crystal seed of 1kg is added；
(2) cooling water about is opened after 40min, continues to cool down, stop cooling to 38~42 DEG C, freezing is opened after crossing 20min
Water (5~7 DEG C) continues to cool down, and stops chilled water when 18~20 DEG C, prepares blowing, and centrifugal dehydration obtains the purity of aluminium oxide
It is 99.82%.
It is pointed out that the technical concepts and features of above-mentioned preferred embodiment only to illustrate the invention, its object is to
Those skilled in the art can understand the contents of the present invention and implements according to this, and the protection of the present invention can not be limited with this
Range.Any equivalent change or modification in accordance with the spirit of the invention should be covered by the protection scope of the present invention.
Claims (5)
1. the method for alumina purifying, it is characterised in that：Using melting crystallizer alumina purifying, the specific steps are：
(1) crystallisation step：It is passed through chilled brine in melting crystallizer external jacket bottom, chilled brine is uniformly in melting crystallizer
Outer wall is in film evaporation device, thick alumina solution is put into melting crystallizer, thick alumina solution is in melting crystallizer inner wall
Falling liquid film flows down, and gradually cools down and crystallizes, and uniform crystal layer is gradually grown on heat-transfer surface, the concentration of crystal layer is higher than melting
The concentration of solution, impurity are gradually enriched in solution in crystallizer；
(2) sweating, fusing：After chilled brine is passed through 30~40min, stops feed, hot water temperature is then adjusted by heat exchanger
Part fusing is carried out to crystal layer, so that the low-melting impurities being mingled in crystal layer fusing is excluded, further purifies crystal.
2. the method for alumina purifying according to claim 1, it is characterised in that：The crystallisation step is specially：First molten
Melt crystallizer external jacket bottom and be passed through chilled brine, temperature is -10 DEG C~-2 DEG C, and chilled brine is uniformly outside melting crystallizer
Wall is in film evaporation device, is then put into thick alumina solution in melting crystallizer, while by melting crystallizer gas-guide tube with 4
~7m3The speed of/min is passed through compressed air into thick alumina solution, is allowed to form the rising of slug flow bubble in crystallizer,
The turbulence of melt, mass transfer enhancement and heat transfer property, alumina solution is caused gradually to be cooled down under melting crystallizer inner wall falling liquid film stream
And crystallize, gradually grow uniform crystal layer on heat-transfer surface, the concentration of crystal layer higher than in melting crystallizer solution it is dense
Degree, impurity are gradually enriched in solution.
3. the method for alumina purifying according to claim 1, it is characterised in that：The sweating, fusing are specially：It controls cold
After jelly brine is passed through 30~40min of time, stop feed, switching warm water tank carries out part fusing, warm water tank water temperature to crystal layer
It it is 88~92 DEG C, warm water is passed through the time as 15~40min；Then switching hot-water cylinder keeps the low-melting impurities being mingled in crystal layer molten
Change and exclude, further purify crystal, hot-water cylinder water temperature is 90~94 DEG C, and hot water is passed through the time as 25~35min.
4. the method for alumina purifying according to claim 1 or claim 2, it is characterised in that：The chilled brine is that calcium chloride is molten
Liquid or sodium chloride solution.
5. the method for alumina purifying according to claim 1 or claim 2, it is characterised in that：The melting crystallizer is vertical row
The falling film melt crystallization device of heat exchange of heat pipe formula.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810322688.3A CN108622923A (en) | 2018-04-11 | 2018-04-11 | The method of alumina purifying |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810322688.3A CN108622923A (en) | 2018-04-11 | 2018-04-11 | The method of alumina purifying |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108622923A true CN108622923A (en) | 2018-10-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810322688.3A Withdrawn CN108622923A (en) | 2018-04-11 | 2018-04-11 | The method of alumina purifying |
Country Status (1)
| Country | Link |
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| CN (1) | CN108622923A (en) |
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2018
- 2018-04-11 CN CN201810322688.3A patent/CN108622923A/en not_active Withdrawn
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| PB01 | Publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20181009 |
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| WW01 | Invention patent application withdrawn after publication |