CN108585010A - A method of preparing pure alpha-aluminum oxide using activated alumina is discarded - Google Patents
A method of preparing pure alpha-aluminum oxide using activated alumina is discarded Download PDFInfo
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- CN108585010A CN108585010A CN201810745907.9A CN201810745907A CN108585010A CN 108585010 A CN108585010 A CN 108585010A CN 201810745907 A CN201810745907 A CN 201810745907A CN 108585010 A CN108585010 A CN 108585010A
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- activated alumina
- purity
- rotary kiln
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- hydrogen peroxide
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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
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
- C01F7/442—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination in presence of a calcination additive
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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
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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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- 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 a kind of high-purity α Al are prepared using discarded activated alumina2O3Method, this method is by discarded activated alumina and α Al2O3After the mixing of crystal seed powder, it is introduced into preheating in rotary kiln tower and preheating is dried, the reaction zone that preheated mixture material enters rotary kiln completes calcination process, and calcining materials discharging to cooler is cooled down, and cooling material obtains α Al by screening2O3.Discarded activated alumina (γ types activated alumina) containing organic anthraquinone etc. and the impurity such as inorganic base during process for prepairng hydrogen peroxide by anthraquinone (hydrogen peroxide) is prepared high-purity α Al by solid phase method by this method2O3Material realizes the recycling of waste and old activated alumina, solves that the waste and old alumina recovery utilization rate generated in existing hydrogen peroxide production process is low, and processing mode is unreasonable, the problems such as resulting in waste of resources.
Description
Technical field
The present invention relates to a kind of discarded activated alumina reuse methods, and in particular to a kind of to utilize anthraquinone production peroxide
Discarded activated alumina (γ types activated alumina) prepares high-purity α-Al by solid phase method during changing hydrogen (hydrogen peroxide)2O3Material
The method of material belongs to waste resource reutilization technology field.
Background technology
Hydrogen peroxide is a kind of important Inorganic Chemicals and fine chemical product, as oxidant, bleaching agent, disinfectant
Etc. being widely used in the fields such as chemical industry, weaving, papermaking, medicine, metallurgy, electronics, agricultural, military affairs and environmental protection.With economical complete
The application field of the fast development of nodularization, hydrogen peroxide is constantly expanded, and the demand of hydrogen peroxide also constantly increases.Anthraquinone preparation is double
Oxygen water is one of the sector the most mature production method in the world at present, and this method is by hydrogenation, oxidation, extraction, purification, rear
Reason and other aided processes composition.With 2- ethyl hydrazine (EAQ) for carrier, heavy aromatics (AR) and trioctyl phosphate (TOP) are mixed
Bonding solvent is configured to working solution, it is passed through together with hydrogen in the hydrogenation bed equipped with catalyst, EAQ is in certain pressure and temperature
Degree is lower and hydrogen carries out hydrogenation, generates corresponding hydrogen anthraquinone (HEAQ), acquired solution is known as hydride.Hydride again with sky
Oxygen in gas carries out oxidation reaction, and hydrogen anthraquinone therein reverts to original anthraquinone, while generating hydrogen peroxide, acquired solution
Referred to as oxidation solution.Using hydrogen peroxide in water and working solution the density contrast of the difference of solubility and working solution and water, use pure water
The hydrogen peroxide in oxidation solution is extracted, aqueous hydrogen peroxide solution (hydrogen peroxide) is obtained.The purified processing of this aqueous solution can be obtained
Hydrogen peroxide product.Working solution (extract liquor) after water extracts, by postprocessing working procedures K2CO3Solution drying and dehydrating decomposes
H2O2With sedimentation separation alkali, then through in carclazyte bed activated alumina absorption except alkali and regeneration degradation product after obtain working solution, then
It recycles.
Active aluminium hydroxide is used for hydride Regenerative beds and carclazyte bed in hydrogen peroxide production process.In hydride Regenerative beds
In effect be regenerate hydride in anthraquinone degradation products, increase working solution in effective anthraquinone content；Work in carclazyte bed
With being regenerating section anthraquinone degradation products and the solution of potassium carbonate in absorption working solution, prevent from, because basicity is excessively high in working solution, making hydrogen
Change catalyst poisoning inactivation.It can be seen that mainly containing the organic matters such as anthraquinone, three pungent fat of sulfuric acid, aromatic hydrocarbons in activated alumina, also
Lye, moisture and other micro substances.These substances make activating oxide internal gutter partly or entirely be blocked, internal structure
Great variety occurs, forms than originally finer and close structure, internal aperture disappears or becomes smaller, and activated alumina is caused to compare table
Area reduces, and with the extension of usage time, the activity of aluminium oxide can continuously decrease, and the aluminium oxide regeneration replaced exists
Certain difficulty.Many Hydrogen Peroxide Production enterprises are not also matched generally all without the regeneration of waste and old activated alumina, retracting device
Solid-waste treatment facility, and this is handled as a kind of Industrial Solid Waste, the huge waste of resource is not only caused, while
Serious pollution can be caused to environment.In recent years, with the rapid raising of hydrogen peroxide production capacity, the reprocessing amount of aluminium oxide is discarded
Increase therewith, in hydrogen dioxide solution production by anthraquinone process technique, hydrogen peroxide yield is the enterprise of 50,000 t/a need to consume activated alumina every year
2000~2500t.Due to being unable to fully using the waste and old activated alumina material generated, severe Environmental Protection Situation in addition, dioxygen
Water industry is faced with huge challenge.
Invention content
For activated alumina is discarded in the prior art, there are ecological environmental pollution, the technical problems such as wasting of resources, this hairs
Bright purpose be to provide it is a kind of by during process for prepairng hydrogen peroxide by anthraquinone (hydrogen peroxide) containing organic anthraquinone etc. and inorganic base
The discarded activated alumina (γ types activated alumina) of equal impurity prepares high-purity α-Al by solid phase method2O3The method of material, should
Method realizes the recycling of waste and old activated alumina, solves the waste and old oxidation generated in existing hydrogen peroxide production process
Alum recovery utilization rate is low, and processing mode is unreasonable, the problems such as resulting in waste of resources.
In order to achieve the above technical purposes, high-purity α-Al being prepared using discarded activated alumina the present invention provides a kind of2O3
Method, this method is by discarded activated alumina and α-Al2O3After crystal seed powder carries out mixing and drying and preheating, in 1200 DEG C
~1400 DEG C of temperature lower calcination processing, it is cooling, it sieves to get α-Al2O3。
Preferred scheme discards activated alumina and α-Al2O3Crystal seed powder mixed proportion meets aluminium oxide in mixed material
Mass percentage content 65~89%, biodiversity degree are 6~20%, and organic matter gross mass degree is 5
~15%, it is 100% metering with mixed material gross mass.
More preferably scheme, the discarded activated alumina include in hydrogen peroxide production process hydride Regenerative beds and/or
Failure activated alumina in carclazyte bed.
Preferred scheme, the calcination processing are realized by rotary kiln；Discarded activated alumina and α-Al2O3Crystal seed powder
After mixing, it is introduced into preheating in rotary kiln tower and preheating is dried, the reaction zone that preheated mixture material enters rotary kiln completes calcining
Process, calcining materials discharging to cooler are cooled down, and cooling material obtains α-Al by screening2O3。
More preferably scheme discards activated alumina and α-Al2O3Crystal seed powder mixed material is in rotary kiln with 70~95
DEG C/m rates are warming up to 1280~1320 DEG C, 1.0~2.0h is kept the temperature, then cool down with 75~100 DEG C/m rates in cooler.It is logical
Cross stringent control heating rate so that alumina material is heated evenly in calcination process, can control the oxidation of γ types well
The phase transition process of aluminium crystal, to improve phase transformation conversion rate, the held for some time under 1300 DEG C or so high temperature can ensure
γ type aluminium oxide is sufficiently converted into α-Al2O3, then by controlling rate of temperature fall appropriate, stablized with ensureing to generate, and grain size
Suitable high-purity α-Al2O3Crystal.
Preferred scheme, the kiln tail ventilation opening negative pressure of rotary kiln is -20~-100Pa in calcination process.It can ensure in kiln
Ventilation and rotary system are closed, play the ability to work of rotary kiln to greatest extent.
α-Al prepared by the present invention2O3The specific surface area of material is low, and heat resistance is strong, good moldability, and crystalline phase is stable, hardness is high,
Good stability of the dimension can be widely used for sizing, amorphous refractory, castable refractory bonding agent, Wear-resistant Sharper, high-purity fire resisting
The products such as fiber and various plastics, glass, ceramics.
Technical scheme of the present invention γ-Al in realizing discarded activated alumina2O3Efficient Conversion is at α-Al2O3Process
In, by adding α-Al2O3Crystal seed powder and calcination temperature is strictly controlled, γ-Al can be greatly improved2O3It is converted to α-
Al2O3Efficiency, improve α-Al2O3Purity.In general, by γ-Al2O3It is converted to α-Al2O3Phase transition process in
It will appear a series of transiens phase, if γ phases are transformed into δ phases at 750 DEG C, be transformed into θ phases when being warming up to 1000 DEG C,
It is transformed into α phases at 1200 DEG C.The present invention makes γ-Al by being calcined under 1200 DEG C of temperatures above2O3It is converted to stable α-
Al2O3, in γ-Al2O3It is converted to α-Al2O3During, improve temperature can significantly improve transformation rate, but can bring as
Crystal grain such as is grown up at the negative effects, and the present invention passes through is added α-Al in discarded active oxidation aluminum feedstock2O3Crystal seed powder, relatively low
At a temperature of realize γ-Al2O3Efficient Conversion, γ-Al can be substantially reduced2O3Phase transformation system energy consumption of reaction, while increasing α-
Al2O3Product purity.
The present invention passes through the addition α-Al in discarded activated alumina2O crystal seed powder, can be bright during solid phase reaction
It is aobvious to reduce γ-Al2O3It is converted to α-Al2O3Reaction activity, α-Al are added in the feed2O3Crystal seed powder can increase phase transformation
The nucleation density of process improves α-Al2O3Conversion ratio.
The utilization of the present invention discards activated alumina and prepares high-purity α-Al2O3Method, it is specific as follows：By anthraquinone production
Fail activated alumina and part α-Al in hydride Regenerative beds and carclazyte bed during hydrogen peroxide2O3After the mixing of crystal seed powder,
Boosted machine enters preheating in rotary kiln tower drying and preheating；Mixed material is driven to enter kiln body master by inclined cylinder of rotary kiln anti-
Area is answered, the technical process constantly completed calcining, decomposed；Material after reaction is by discharge cover discharging to cooler, through cooling, sieve
Material after point is high-purity α-Al2O3Material；Tail gas after reaction is through denitrating system, cyclone dust removal+bag-type dust removal system from tail
Gas blowdown stack is discharged.
In the calcination process of the present invention, rotary kiln is using natural gas as combustion gas, while with the organic matter in air and material
For combustion adjuvant, calcined in 1200 DEG C~1400 DEG C of high temperature rotary kiln, material stopped in rotary kiln total time be 3~
5h obtains high-purity α-Al after cooling through screening2O3Material.Material residence time in rotary kiln is more preferably 4h.Not only may be used
To improve α-Al2O3Product purity, and avoid increasing equipment investment and operating cost.
Preheating is dried to material in the present invention, and the temperature of preheating is generally 400 DEG C or so.Calcining materials are generally cooled to
200 DEG C or less.
The rotary kiln and cooler that the present invention uses do not require particularly, are realized using existing common device.Such as this
Invention is illustrated by taking straight tube rotary kiln as an example.The barrel diameter of rotary kiln is 2200mm, barrel lenght 45000mm, gradient
It is preferred that 3%.When work, 1~3r/min of rotating speed.Cooler uses single cylinder cooling machine, and specification isRotating speed 5 when work
~8r/min.
Compared with the prior art, technical scheme of the present invention has the advantage that effect：
(1) present invention prepares the higher high-purity α-of added value using industrially discarded waste and old activated alumina for the first time
Al2O3Material has considerable economic benefit, it is possible to reduce waste to waste and old aluminium oxide and is conducive to environmental protection.
(2) present invention in waste and old active oxidation aluminum feedstock by being added α-Al2O3Crystal seed powder can not only reduce height
Material phase transformation system energy consumption of reaction during warm solid phase reaction, and γ-Al can be improved2O3Conversion ratio increases α-Al2O3Production
Product purity.
(3) waste and old activated alumina of the invention is converted to high-purity α-Al2O3The process of material realized by single step reaction,
It is easy to operate, and existing conventional equipment device can be borrowed, it is at low cost, be conducive to industrialized production and application.
(4) present invention directly can prepare high-purity α-by high temperature solid state reaction using waste and old active oxidation aluminum feedstock
Al2O3, it is not organic in by waste and old activated alumina to be influenced with inorganic impurity, it is high-purity more than 96% or more to directly obtain purity
Product.
(5) high-purity α-Al that the present invention is produced using waste and old activated alumina as raw material2O3Material has good heat-resisting
Performance and slag resistance, pollution-free, service life is long, has good reparation, regeneration function and extensive purposes range.
Description of the drawings
【Fig. 1】For waste and old activated alumina in calcination process variation feelings of the temperature of charge in rotary kiln and cooler
Condition.
【Fig. 2】It is waste and old activated alumina in 2% (w/w) α-Al2O3Under the different calcination conditions of crystal seed powder additive amount
α-the Al arrived2O3Product content situation.
【Fig. 3】For the process flow chart of the present invention.
Specific implementation mode
Technical scheme of the present invention is further described below by way of specific embodiment, rather than limits present invention power
The protection domain that profit requires.
In the present invention, it if not refering in particular to, all devices and is commercially available using medicament or the industry is common, under
It is unless otherwise instructed this field conventional method to state the method implemented in example.
It presses following operation and implements in following example 1~4：
1) raw material sources：Raw material sources are in Hydrogen Peroxide Production factory A：Hydride Regenerative beds and carclazyte bed in Hydrogen Peroxide Production
In the waste and old activated alumina of failure, average grain diameter 2mm.
2) equipment：Using straight tube rotary kiln, barrel diameter 2200mm, barrel lenght 45000mm, gradient 3%, rotating speed 2r/
min；Cooler uses single cylinder cooling machine, specification preferredRotating speed 6r/min, residence time 30min.
3) calcination processing process：By the boosted machine of raw material enter preheating in rotary kiln tower drying, by rotary-drum furnace animal material into
Enter kiln body reaction zone, passes through the chemically and physically process such as dry, preheating, calcining, cooling, the high-purity α-generated after reaction successively
Al2O3Material enters screw lifter after the rapid cooling down of cooler, most separates material through Vibration Screen afterwards.What regeneration obtained
High-purity α-Al2O3Material product test result is shown in Table 1.Tail gas after reaction is through denitrating system, cyclone dust removal+bag-type dust removal system
It is discharged from exhaust emissions chimney.
Embodiment 1
By adding 2% (w/w) α-Al2O3Crystal seed powder so that moisture is 10% in raw material, and total organic content is
6%, alumina content 81%；Material is warming up to 1300 DEG C in rotary kiln with 95 DEG C/m rates, and high temperature section soaking time is 2
Hour, total residence time 4h；Rotary kiln inlet pressure is 3Pa, and flue-gas temperature is 360 DEG C, rotary kiln air pressure -31Pa,
Flue-gas temperature is 560 DEG C, and material enters the rate cooling with 90 DEG C/m of highest, discharging in cooler.
Embodiment 2
By adding 2.5% (w/w) α-Al2O3Crystal seed powder so that moisture is 8% in raw material, total organic content
It is 5%, alumina content 84%；Material is heated up 1200 DEG C in rotary kiln with 85 DEG C/m rates, and high temperature section soaking time is 2
Hour, total residence time 4h；Rotary kiln inlet pressure is 5Pa, and flue-gas temperature is 340 DEG C, rotary kiln air pressure -32Pa,
Flue-gas temperature is 540 DEG C, and material enters the rate cooling with 90 DEG C/m of highest, discharging in cooler.
Embodiment 3
By adding 2% (w/w) α-Al2O3Crystal seed powder so that moisture is 10% in raw material, and total organic content is
6%, alumina content 81%；Material is heated up 1200 DEG C in rotary kiln with 85 DEG C/m rates, and high temperature section soaking time is 2 small
When, calcination reaction temperature is 1200 DEG C, total residence time 4h；Rotary kiln inlet pressure is 3Pa, and flue-gas temperature is 350 DEG C, is returned
Rotary kiln kiln tail air pressure -32Pa, flue-gas temperature are 545 DEG C, and material enters the rate cooling with 90 DEG C/m of highest in cooler, goes out
Material.
Embodiment 4
By adding 2% (w/w) α-Al2O3Crystal seed powder so that moisture is 10% in raw material, and total organic content is
6%, alumina content 81%；Material is heated up 1300 DEG C in rotary kiln with 95 DEG C/m rates, and high temperature section soaking time is 1.5
Hour, total residence time 3.5h；Rotary kiln inlet pressure is 4Pa, and flue-gas temperature is 365 DEG C, rotary kiln air pressure-
31Pa, flue-gas temperature are 554 DEG C, and material enters the rate cooling with 90 DEG C/m of highest, discharging in cooler.
High-purity α-Al prepared by 1 Examples 1 to 4 of table2O3Material physico-chemical property is analyzed
Claims (6)
1. a kind of preparing high-purity α-Al using discarded activated alumina2O3Method, it is characterised in that：By discarded activated alumina
With α-Al2O3It after crystal seed powder carries out mixing and drying and preheating, is handled in 1200 DEG C~1400 DEG C temperature lower calcinations, cooling, sieve
Divide to get α-Al2O3。
2. a kind of utilization according to claim 1 discards activated alumina and prepares high-purity α-Al2O3Method, feature exists
In：Discarded activated alumina and α-Al2O3Crystal seed powder mixed proportion meets quality of alumina degree 65 in mixed material
~89%, biodiversity degree is 6~20%, and organic matter gross mass degree is 5~15%.
3. a kind of utilization according to claim 2 discards activated alumina and prepares high-purity α-Al2O3Method, feature exists
In：The discarded activated alumina includes the failure activity in hydride Regenerative beds and/or carclazyte bed in hydrogen peroxide production process
Aluminium oxide.
4. preparing high-purity α-Al using discarded activated alumina according to claims 1 to 3 any one of them is a kind of2O3Method,
It is characterized in that：The calcination processing is realized by rotary kiln；Discarded activated alumina and α-Al2O3After the mixing of crystal seed powder, first
Preheating is dried into preheating in rotary kiln tower, the reaction zone that preheated mixture material enters rotary kiln completes calcination process, calcining
Material discharging to cooler is cooled down, and cooling material obtains α-Al by screening2O3。
5. a kind of utilization according to claim 4 discards activated alumina and prepares high-purity α-Al2O3Method, feature exists
In：Discarded activated alumina and α-Al2O3Crystal seed powder mixed material is warming up to 1280 in rotary kiln with 70~95 DEG C/m rates
~1320 DEG C, 1.0~2.0h is kept the temperature, then cool down with 75~100 DEG C/m rates in cooler.
6. a kind of utilization according to claim 4 discards activated alumina and prepares high-purity α-Al2O3Method, feature exists
In：The kiln tail ventilation opening negative pressure of rotary kiln is -20~-100Pa in calcination process.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810745907.9A CN108585010A (en) | 2018-07-09 | 2018-07-09 | A method of preparing pure alpha-aluminum oxide using activated alumina is discarded |
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| CN201810745907.9A CN108585010A (en) | 2018-07-09 | 2018-07-09 | A method of preparing pure alpha-aluminum oxide using activated alumina is discarded |
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ID=63615203
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114804186A (en) * | 2022-05-16 | 2022-07-29 | 吴江市威士达铜业科技有限公司 | Production method and production device of copper oxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1834016A (en) * | 2005-03-18 | 2006-09-20 | 住友化学株式会社 | Process for producing fine alpha-alumina particles |
| CN1919737A (en) * | 2005-08-26 | 2007-02-28 | 大连路明纳米材料有限公司 | Method of preparing good dispersion and high-purity ultra-fine alpha-Al2O3 |
-
2018
- 2018-07-09 CN CN201810745907.9A patent/CN108585010A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1834016A (en) * | 2005-03-18 | 2006-09-20 | 住友化学株式会社 | Process for producing fine alpha-alumina particles |
| CN1919737A (en) * | 2005-08-26 | 2007-02-28 | 大连路明纳米材料有限公司 | Method of preparing good dispersion and high-purity ultra-fine alpha-Al2O3 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114804186A (en) * | 2022-05-16 | 2022-07-29 | 吴江市威士达铜业科技有限公司 | Production method and production device of copper oxide |
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Application publication date: 20180928 |