CN106830031A - The production method of high purity nanometer alumina - Google Patents
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- CN106830031A CN106830031A CN201710207755.2A CN201710207755A CN106830031A CN 106830031 A CN106830031 A CN 106830031A CN 201710207755 A CN201710207755 A CN 201710207755A CN 106830031 A CN106830031 A CN 106830031A
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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
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
- C01F7/306—Thermal decomposition of hydrated chlorides, e.g. of aluminium trichloride hexahydrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of production method of high purity nanometer alumina.With aluminum sulfate as silicon source, ammonium carbonate is precipitating reagent to this method, and low temperature liquid phase synthesis adds dispersant to prevent from reuniting, and by being transferred to distillation still after press filtration, carries out alcohol and sloughs moisture with the azeotropic distillation of water, and powder is carried out into high-temperature calcination at 900 1200 DEG C obtains α Al2O3Powder, packaging of finally weighing.The production method of the high purity nanometer alumina has the advantages that product purity high, process is simple, low cost, pollution-free.
Description
Technical field
The present invention relates to inorganic ultra-pure nano-powder preparing technical field, and in particular to a kind of high purity nanometer alumina
Production method.
Background technology
High purity nanometer alumina has hardness high, good stability of the dimension, superior performance, can be used as coating, rubber, plastics resistance to
Mill hardening agent, fluorescent material, lithium battery diaphragm coating material, anode material of lithium battery additive, precise polished powder, Sapphire Substrate
Deng.
The method of current domestic industry production high purity nanometer alumina mainly has two major classes, and a class is solid-phase pyrolysis, one
Class is Liquid-phase hydrolysis.Solid phase pyrolysis is mostly to be improved on the basis of Bayer process, and the silicon source of Liquid-phase hydrolysis is divided into inorganic
Aluminium salt and organic aluminium salt, current aluminium alcoholates salt hydrolysis are the important methods for producing ultra-pure nano aluminium oxide, in order to control to be managed
Think product, the method also improved under everybody way always before continuity, such as patent announcement number be CN105948090A,
Method disclosed in the patents such as CN105984891A, CN102874854B.It is also a kind of important method for liquid-phase precipitation method,
Patent announcement number is to disclose aluminum sulfate and alkali lye sluggish precipitation prepares the side of aluminium hydroxide in patent described in CN1285510C
Method, being disclosed in patent described in patent announcement CN1298630C can be lived using alum and ammonium carbonate with prepares coating
Property nano aluminium oxide, and in patent described in patent announcement CN 100473610C in above-mentioned patent change technique and precipitating reagent
Fibrous nano aluminum oxide can be obtained, patent announcement CN101391788A is disclosed using alum and urea in urase
Homogeneous precipitation obtains alumina powder for polishing solution under catalytic action, above-mentioned in patent described in patent announcement ZL103693664B
Ammoniacal liquor is used in patent instead as precipitating reagent, adds dispersant also to obtain polishing aluminum oxide.Patent announcement CN105060324A,
Aluminum nitrate is also served as into silicon source, urea, hydrogen-oxygen in patent described in CN103910369B, CN104708009A and CN103787394B
Changing sodium or ammonium hydrogen carbonate as precipitating reagent react obtaining nano aluminium oxide.Aluminum oxide prepared by these liquid precipitations is pure
Degree is not high, and some particle diameters are larger.Related process is confined to laboratory, without related amplification test.Current high-purity nm oxygen
The preparation for changing aluminium predominantly stays in the experimental exploration stage, and the technological process for exploring suitable industrialized production is very urgent.It is high
Pure nano aluminium oxide is more with expensive alkoxide raw material, and technique is relative complex, and scale is smaller, relatively costly, seriously constrains
Its industrialization process.
The content of the invention
To overcome the shortcomings of in prior art, it is an object of the invention to provide a kind of simple production process, cost is relatively low
High purity nanometer alumina industrialized preparing process.
Technical scheme is as follows：
(1) dispensing
1. a kind of industrialized preparing process of high purity nanometer alumina, it is characterised in that：It is including step as described below：
(1) dispensing
Inorganic aluminate and dispersant are dissolved in high purity water, concentration are made into and are the solution B of 0.2~0.6mol/L, wherein dividing
Powder content is 1~6wt%；Alkali lye and dispersant are dissolved in high purity water, the solution A that concentration is 0.6~1.2mol/L is made into,
Wherein dispersant is 1~6wt%.
(2) liquid phase synthesis
First by solution A by bag filter, in pumping into main reaction kettle, start stirring, add high purity water adjust pH value be 9~
10, then by solution B by bag filter, reaction is made solution C in 1~3 hour in pumping into main reaction kettle.
(3) pressure filtration washing
Solution C is pumped into diaphragm filter press, high-purity water washing is used, foreign ion is removed, filter cake is obtained.
(4) azeotropic distillation dehydration
It is transferred in distillation still when cake moisture is controlled into 5~20wt%, pumping into the alcohol for steaming again carries out vacuum distillation,
Control temperature, cooling for reflux；After the completion of dehydration, temperature rises lasting backflow, steams alcohol recovery, obtains fluffy powder.
(5) calcine
Powder is placed in corundum crucible with cover, is put in furnace chamber, temperature programming, then in 900~1200 DEG C constant temperature 1~
3 hours, high purity nanometer alumina is obtained, purity is 99.99~99.999%.
Further technical scheme is that the flow velocity for pumping into main reaction kettle of solution B is in 1~4m3/ described in step (2)
h。
Further technical scheme is, the alcohol for steaming again described in step (4) is butanol or amylalcohol, the filter cake and institute
The consumption volume ratio for stating the alcohol for steaming again is 1：10~1：20.
Further technical scheme is, inorganic aluminate is high-purity sulphuric acid aluminium or aluminum nitrate in the step (1), its
Purity >=99.9%；The alkali lye be high purity sodium hydroxide, ammoniacal liquor, ammonium hydrogen carbonate or ammonium carbonate in one kind, its purity >=
99.9%.
Further technical scheme is, the high purity water is pure water that resistivity is 15~18 megaohms.
Further technical scheme is, the dispersant be PEG400, Macrogol 600, polyethylene glycol-800,
One or more in cetomacrogol 1000, polyethylene glycol 2000.
Further technical scheme is, in the step (2) bag filter be used to filtering out solution A, B it is insoluble
Impurity.
Further technical scheme is that control diaphragm pressure is in 0.1~0.4MPa, wash time in the step (3)
In 10~30min.
Further technical scheme is that the vacuum in the step (4) in distillation still is 0.04~0.08MPa, temperature
50~80 DEG C, return time 3-7 hours of degree.
Further technical scheme is that it is to rise to 500 with 10 DEG C/min of heating rate that step (5) Program heats up
DEG C, then 900 DEG C are risen to 15 DEG C/min, 1100 DEG C then are risen to 5 DEG C/min, then constant temperature 1~3 hour.
The invention reside in by improving the existing technique for preparing high purity nanometer alumina, a kind of suitable industrialized production is invented
Method.The nano aluminium oxide that purity is up to more than 99.992 can be obtained using inorganic aluminate liquid phase reactor, this process is simple is easy
Operation, tail gas recycle, reduce discharging of waste liquid, are that environmental protection is done one's bit, and reduce the expense of business processes waste water, economize on resources
Reduces cost, this process recovery ratio is higher.
Brief description of the drawings
Fig. 1 is the process chart of high purity nanometer alumina synthetic method proposed by the present invention.
Specific embodiment
The invention discloses a kind of industrialized preparing process of high purity nanometer alumina, as shown in Figure 1.It includes following institute
Stating step is：
(1) dispensing
Inorganic aluminate and dispersant are dissolved in high purity water, concentration are made into and are the solution B of 0.2~0.6mol/L, wherein dividing
Powder content is 1~6wt%；Alkali lye and dispersant are dissolved in high purity water, the solution A that concentration is 0.6~1.2mol/L is made into,
Wherein dispersant is 1~6wt%.
(2) liquid phase synthesis
First by solution A by bag filter, in pumping into main reaction kettle, start stirring, add high purity water adjust pH value be 9~
10, then by solution B by bag filter, reaction is made solution C in 1~3 hour in pumping into main reaction kettle.
(3) pressure filtration washing
Solution C is pumped into diaphragm filter press, high-purity water washing is used, foreign ion is removed, filter cake is obtained.
(4) azeotropic distillation dehydration
It is transferred in distillation still when cake moisture is controlled into 5~20wt%, pumping into the alcohol for steaming again carries out vacuum distillation,
Control temperature, cooling for reflux；After the completion of dehydration, temperature rises lasting backflow, steams alcohol recovery, obtains fluffy powder.
(5) calcine
Powder is placed in corundum crucible with cover, is put in furnace chamber, temperature programming, then in 900~1200 DEG C constant temperature 1~
3 hours, high purity nanometer alumina is obtained, purity is 99.99~99.999%.
Preferably, the flow velocity for pumping into main reaction kettle of solution B described in step (2) is in 1~4m3/h.
Preferably, the alcohol for steaming again described in step (4) is butanol or amylalcohol, the use of the filter cake and the alcohol of the heavy steaming
Amount volume ratio is 1：10~1：20.
Preferably, inorganic aluminate is high-purity sulphuric acid aluminium or aluminum nitrate, its purity >=99.9% in the step (1)；Institute
It is the one kind in high purity sodium hydroxide, ammoniacal liquor, ammonium hydrogen carbonate or ammonium carbonate, its purity >=99.9% to state alkali lye.
Preferably, the high purity water is pure water that resistivity is 15~18 megaohms.
Preferably, the dispersant be PEG400, Macrogol 600, polyethylene glycol-800, cetomacrogol 1000,
One or more in polyethylene glycol 2000.
Preferably, bag filter is used to filter out the insoluble impurities of solution A, B in the step (2).
Preferably, control diaphragm pressure in 0.1~0.4MPa in the step (3), wash time is in 10~30min.
Preferably, the vacuum in the step (4) in distillation still is 0.04~0.08MPa, 50~80 DEG C of temperature, backflow
Time 3-7 hours.
Preferably, it is to rise to 500 DEG C with 10 DEG C/min of heating rate that step (5) Program heats up, then with 15 DEG C/
Min rises to 900 DEG C, then rises to 1100 DEG C with 5 DEG C/min, then constant temperature 1~3 hour.
Embodiment 1：The preparation of α-Al2O3
300kg ammonium carbonates (99.9%) and 100kgPEG2000 (99.9%) are dissolved in 2m3High purity water, through bag type filtering
Device, vacuum is evacuated in main reaction kettle.500kg aluminum sulfate octadecahydrates and 100kg PEG2000 (99.9%) are dissolved in 2m3It is high-purity
Water, through bag filter, pumps into main reaction kettle, and flow velocity is 2.0m3/ h, is stirred at room temperature reaction 3h, with 0.5MPa pressure by part
Slurry obtains filter cake by diaphragm filter press, and diaphragm pressure is controlled in 0.25MPa, and be transferred to for filter cake by high-purity water washing 30min
In azeotropic distillation kettle, 10 times of n-butanols of volume are added, vacuum distillation is carried out with 0.06MPa pressure, azeotropic mixture is removed substantially after 3h
Only, continue to flow back 5 hours, n-butanol is steamed successively, obtain fluffy powder.Powder is placed in corundum crucible with cover, program control
Under temperature, 1150 DEG C of insulation 2h obtain uniform particle sizes, and purity is 99.995% α-Al2O3 powder.
Embodiment 2：The preparation of α-Al2O3
250kg ammonium hydrogen carbonate (99.9%) and 100kgPEG2000 (99.9%) are dissolved in 2m3High purity water, through bag type filtering
Device, vacuum is evacuated in main reaction kettle.500kg aluminum sulfate octadecahydrates and 100kg PEG2000 (99.9%) are dissolved in 2m3 high-purity
Water, through bag filter, pumps into main reaction kettle, and flow velocity is 2.0m3/ h, is stirred at room temperature reaction 3h, with 0.5MPa pressure by part
Slurry obtains filter cake by diaphragm filter press, and diaphragm pressure is controlled in 0.15MPa, and be transferred to for filter cake by high-purity water washing 20min
In azeotropic distillation kettle, 10 times of n-butanols of volume are added, vacuum distillation is carried out with 0.06MPa pressure, azeotropic mixture is removed substantially after 3h
Only, continue to flow back 5 hours, n-butanol is steamed successively, obtain fluffy powder.Powder is placed in corundum crucible with cover, program control
Under temperature, 1100 DEG C of insulation 2h obtain uniform particle sizes, and purity is 99.993% α-Al2O3 powder.
Embodiment 3：The preparation of α-Al2O3
150kg ammonium carbonates (99.9%) and 50kgPEG2000 (99.9%) are dissolved in 2m3High purity water, through bag filter,
Vacuum is evacuated in main reaction kettle.The water aluminum nitrates of 140kg nine and 50kg PEG2000 (99.9%) are dissolved in 2m3High purity water, through bag
Formula filter, pumps into main reaction kettle, and flow velocity is 2.0m3/ h, is stirred at room temperature reaction 3h, is passed through part size with 0.5MPa pressure
Diaphragm filter press obtains filter cake, and diaphragm pressure is controlled in 0.25MPa, and filter cake is transferred to azeotropic distillation by high-purity water washing 30min
In kettle, 10 times of n-butanols of volume are added, vacuum distillation is carried out with 0.06MPa pressure, azeotropic mixture is substantially cleared after 3h, continues back
Stream 5 hours, steams n-butanol successively, obtains fluffy powder.Powder is placed in corundum crucible with cover, under temperature programmed control, 1100
DEG C insulation 2h, obtain uniform particle sizes, purity is 99.995% α-Al2O3 powder.
Embodiment 4：The preparation of α-Al2O3
125kg ammonium hydrogen carbonate (99.9%) and 100kgPEG2000 (99.9%) are dissolved in 2m3High purity water, through bag type filtering
Device, vacuum is evacuated in main reaction kettle.The water aluminum nitrates of 140kg nine and 100kg PEG2000 (99.9%) are dissolved in 2m3High purity water,
Through bag filter, main reaction kettle is pumped into, flow velocity is 2.0m3/ h, is stirred at room temperature reaction 3h, is starched part with 0.5MPa pressure
Material obtains filter cake by diaphragm filter press, and diaphragm pressure is controlled in 0.3MPa, and be transferred to filter cake altogether by high-purity water washing 30min
In boiling distillation still, 10 times of n-butanols of volume are added, vacuum distillation are carried out with 0.06MPa pressure, azeotropic mixture is substantially cleared after 3h,
Continue to flow back 5 hours, n-butanol is steamed successively, obtain fluffy powder.Powder is placed in corundum crucible with cover, temperature programmed control
Under, 1150 DEG C of insulation 3h obtain uniform particle sizes, and purity is 99.994% α-Al2O3 powder.
Embodiment 5：The preparation of α-Al2O3
125kg ammonium hydrogen carbonate (99.9%) and 100kgPEG2000 (99.9%) are dissolved in 2m3High purity water, through bag type filtering
Device, vacuum is evacuated in main reaction kettle.The water aluminum nitrates of 140kg nine and 100kg PEG2000 (99.9%) are dissolved in 2m3High purity water,
Through bag filter, main reaction kettle is pumped into, flow velocity is 2.0m3/ h, is stirred at room temperature reaction 3h, with 0.5MPa pressure by part size
Filter cake is obtained by diaphragm filter press, diaphragm pressure is controlled in 0.3MPa, and filter cake is transferred to azeotropic by high-purity water washing 30min
In distillation still, 10 times of n-amyl alcohols of volume are added, vacuum distillation is carried out with 0.06MPa pressure, azeotropic mixture is substantially cleared after 3h, after
Continuous backflow 5 hours, steams n-butanol successively, obtains fluffy powder.Powder is placed in corundum crucible with cover, under temperature programmed control,
1150 DEG C of insulation 3h, obtain uniform particle sizes, and purity is 99.992% α-Al2O3 powder.
Embodiment 6：The preparation of α-Al2O3
250kg ammonium hydrogen carbonate (99.9%) and 100kgPEG2000 (99.9%) are dissolved in 2m3High purity water, through bag type filtering
Device, vacuum is evacuated in main reaction kettle.500kg aluminum sulfate octadecahydrates and 100kg PEG2000 (99.9%) are dissolved in 2m3It is high-purity
Water, through bag filter, pumps into main reaction kettle, and flow velocity is 2.0m3/ h, is stirred at room temperature reaction 3h, with 0.5MPa pressure by part
Slurry obtains filter cake by diaphragm filter press, and diaphragm pressure is controlled in 0.15MPa, and be transferred to for filter cake by high-purity water washing 20min
In azeotropic distillation kettle, 10 times of n-amyl alcohols of volume are added, vacuum distillation is carried out with 0.06MPa pressure, azeotropic mixture is removed substantially after 3h
Only, continue to flow back 5 hours, n-butanol is steamed successively, obtain fluffy powder.Powder is placed in corundum crucible with cover, program control
Under temperature, 1200 DEG C of insulation 2h obtain uniform particle sizes, and purity is 99.994% α-Al2O3 powder.
The invention reside in by improving the existing technique for preparing high purity nanometer alumina, a kind of suitable industrialized production is invented
Method.The nano aluminium oxide that purity is up to more than 99.992 can be obtained using inorganic aluminate liquid phase reactor, this process is simple is easy
Operation, tail gas recycle, reduce discharging of waste liquid, are that environmental protection is done one's bit, and reduce the expense of business processes waste water, economize on resources
Reduces cost, this process recovery ratio is higher.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to model of the invention
Enclose and be defined, various modifications and improvement, in the protection domain that claims of the present invention determines.
Claims (10)
1. a kind of industrialized preparing process of high purity nanometer alumina, it is characterised in that：It is including step as described below：
(1) dispensing
Inorganic aluminate and dispersant are dissolved in high purity water, the solution B that concentration is 0.2~0.6mol/L, wherein dispersant is made into
Content is 1~6wt%；Alkali lye and dispersant are dissolved in high purity water, the solution A that concentration is 0.6~1.2mol/L is made into, wherein
Dispersant is 1~6wt%；
(2) liquid phase synthesis
First by solution A by bag filter, pump into main reaction kettle, start stirring, it is 9~10 to add high purity water to adjust pH value,
Again by solution B by bag filter, reaction is made solution C in 1~3 hour in pumping into main reaction kettle；
(3) pressure filtration washing
Solution C is pumped into diaphragm filter press, high-purity water washing is used, foreign ion is removed, filter cake is obtained；
(4) azeotropic distillation dehydration
It is transferred in distillation still when cake moisture is controlled into 5~20wt%, pumping into the alcohol for steaming again carries out vacuum distillation, is controlled
Temperature, cooling for reflux；After the completion of dehydration, temperature rises lasting backflow, steams alcohol recovery, obtains fluffy powder；
(5) calcine
Powder is placed in corundum crucible with cover, is put in furnace chamber, temperature programming, then constant temperature 1~3 is small in 900~1200 DEG C
When, high purity nanometer alumina is obtained, purity is 99.99~99.999%.
2. the production method of high purity nanometer alumina according to claim 1, it is characterised in that：It is molten described in step (2)
The flow velocity for pumping into main reaction kettle of liquid B is in 1~4m3/h。
3. the production method of high purity nanometer alumina according to claim 1, it is characterised in that：Described in step (4)
The alcohol for steaming again is butanol or amylalcohol, and the filter cake is 1 with the consumption volume ratio of the alcohol of the heavy steaming：10~1：20.
4. the production method of high purity nanometer alumina according to claim 1, it is characterised in that：Nothing in the step (1)
Machine aluminium salt is high-purity sulphuric acid aluminium or aluminum nitrate, its purity >=99.9%；The alkali lye is high purity sodium hydroxide, ammoniacal liquor, carbonic acid
One kind in hydrogen ammonium or ammonium carbonate, its purity >=99.9%.
5. the production method of high purity nanometer alumina according to claim 1, it is characterised in that：The high purity water is resistance
Rate is 15~18 megaohms of pure water.
6. the production method of high purity nanometer alumina according to claim 1, it is characterised in that：The dispersant is poly- second
One or more in glycol 400, Macrogol 600, polyethylene glycol-800, cetomacrogol 1000, polyethylene glycol 2000.
7. the production method of high purity nanometer alumina according to claim 1, it is characterised in that：Bag in the step (2)
Formula filter is used to filter out the insoluble impurities of solution A, B.
8. the production method of high purity nanometer alumina according to claim 1, it is characterised in that：Control in the step (3)
, in 0.1~0.4MPa, wash time is in 10~30min for diaphragm pressure processed.
9. the production method of high purity nanometer alumina according to claim 1, it is characterised in that：Steamed in the step (4)
The vacuum in kettle is evaporated for 0.04~0.08MPa, 50~80 DEG C, return time 3-7 hours of temperature.
10. the production method of high purity nanometer alumina according to claim 1, it is characterised in that：Step (5) intermediate range
It is to rise to 500 DEG C with 10 DEG C/min of heating rate that sequence heats up, then rises to 900 DEG C with 15 DEG C/min, is then risen to 5 DEG C/min
1100 DEG C, then constant temperature 1~3 hour.
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| CN107758718A (en) * | 2017-11-17 | 2018-03-06 | 宁波普莱斯帝金属制品有限公司 | A kind of method that calcium carbonate superfine powder nano-powder is prepared with calcite |
| CN109534378A (en) * | 2018-11-27 | 2019-03-29 | 东华大学 | A kind of preparation method of anti-hard aggregation nano alumina particles |
| CN109534379A (en) * | 2019-01-09 | 2019-03-29 | 上海大学(浙江·嘉兴)新兴产业研究院 | A kind of nano-level sphere γ-Al2O3The low cost preparation method of powder |
| CN113698183A (en) * | 2021-08-27 | 2021-11-26 | 湖州南木纳米科技有限公司 | Carbon-coated alumina ceramic material and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107758718A (en) * | 2017-11-17 | 2018-03-06 | 宁波普莱斯帝金属制品有限公司 | A kind of method that calcium carbonate superfine powder nano-powder is prepared with calcite |
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| CN109534379A (en) * | 2019-01-09 | 2019-03-29 | 上海大学(浙江·嘉兴)新兴产业研究院 | A kind of nano-level sphere γ-Al2O3The low cost preparation method of powder |
| CN113698183A (en) * | 2021-08-27 | 2021-11-26 | 湖州南木纳米科技有限公司 | Carbon-coated alumina ceramic material and preparation method and application thereof |
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