CN105948090A - Ultra-pure nano-alumina green synthesis method and industrialization device - Google Patents
Ultra-pure nano-alumina green synthesis method and industrialization device Download PDFInfo
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- CN105948090A CN105948090A CN201610410951.5A CN201610410951A CN105948090A CN 105948090 A CN105948090 A CN 105948090A CN 201610410951 A CN201610410951 A CN 201610410951A CN 105948090 A CN105948090 A CN 105948090A
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- isopropanol
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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
- C01F7/42—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation
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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
Abstract
The invention provides an ultra-pure nano-alumina green synthesis method. The method comprises the steps that high purity aluminum, isopropanol, a catalyst, an iron removal agent and a silicon removal agent are injected into a synthetic reaction kettle, a synthetic reaction is conducted, and liquid aluminum isopropoxide is obtained; liquid ultra-pure aluminum isopropoxide is obtained through evaporation filtration; liquid ultra-pure aluminum isopropoxide is slowly injected into a hydrolysis ageing drying tank, hydrolysate is slowly added simultaneously for a hydrolysis reaction, algeldrate is obtained, and ultra-pure aluminum hydroxide powder is obtained through ageing drying; calcination is conducted, and Al2O3 powder is obtained; smashing is conducted, and then measuring and packing are conducted; isopropanol tail gas produced in the above-mentioned steps is subjected to recycle disposal through a recovery device, and obtained liquid isopropanol serves as the isopropanol raw material in the first step. The invention further provides a green synthesis industrialization device of ultra-pure nano-alumina. The green synthesis industrialization device is low in cost, free of environmental pollution and capable of being widely applied to the field of ultra-pure nano-alumina production.
Description
Technical field
The present invention relates to inorganic ultra-pure nano-powder preparing technical field, be specifically related to purity ＞ 99.9% and with
On high-purity aluminium ingot prepare ultra high purity nitric oxide aluminium powder body green synthesis method and industrialization device.
Background technology
Ultra-pure nano aluminium oxide not only has common aluminium oxide fusing point height, refractoriness is high, mechanical behavior under high temperature is good, electric
Good insulating, the characteristic that acid and alkali-resistance erosion performance is strong and hardness is high, also have quantum size effect, small-size effect, surface effect
Should nano material distinctive character many with macro quanta tunnel effect etc., be therefore widely used in a lot of fields.Ultra-pure
The preparation method of nano aluminium oxide has a variety of, and the powder characteristics that current vapor phase method is prepared is good, but cost is the highest；Aluminium alcoholates is molten
Sol-gel prepares ultra-pure nano aluminium oxide mild condition, and product purity is high, and epigranular, is to prepare ultra-pure receiving at present
A kind of most potential method of rice aluminium oxide.But the aluminium alcoholates sol-gal process of routine is directly with aluminium alcoholates as raw material, production cost
The highest, and react, distill, all will produce substantial amounts of alcohol during separation etc., directly discharge is by serious environment pollution.How to drop
Low production cost, reduce the pollution to environment in production process, it is achieved ultra-pure nano alumina powder jointed green syt is to receive
The alumina powder jointed key that can be used widely further of rice.Scholars are to ultra-pure nanometer A1 at present2O3Research main
Concentrate on laboratory preparation on, to the Cost Problems in ultra-pure nano alumina powder jointed commercial process, environmental problem,
It is less that industrialization device is studied.The problem such as serious additionally, ultra-pure nano alumina powder jointed pattern is difficult to control to and reunites
It is to limit ultra-pure nano alumina powder jointed further wide variety of technical barrier at present.
Summary of the invention
For overcoming above technical deficiency, on study for reference ancestor and colleague's scientific achievement and the basis about patent
On, the present invention proposes that a kind of cost is relatively low, ultra-pure nano aluminium oxide green synthesis method that environmental pollution is less and industry
Gasifying device.
In order to solve the problems referred to above, the technical solution used in the present invention is: a kind of ultra-pure nano aluminium oxide green syt
Method, its processing step is: a kind of ultra-pure nano aluminium oxide green synthesis method, and its processing step is:
(1) synthesis technique: by rafifinal bits and isopropanol, joins the reactor heated by bottom and upper condensator forms
In synthetic reaction tower, add catalyst, iron removing reagent, desiliconizing agent post-heating, isopropanol and aluminum generation synthetic reaction, generate gaseous state different
Aluminum tripropoxide；Gaseous state aluminum isopropylate. enters condenser, after condensed device is cooled to liquid aluminum isopropylate., is back to described reactor
In, the most ceaselessly evaporation-condensation-backflow, complete synthetic reaction, final aluminum bits and isopropanol generate liquid isopropanol completely
Aluminum；
(2) distilation technique: liquid aluminum isopropylate. is injected in distillating still and flash to aluminum isopropylate. steam, after entering splice jug
Become liquid high puring aluminium isopropoxide, then liquid high puring aluminium isopropoxide is crossed at a temperature of 160 DEG C nano ceramics Membrane filtering machine, filter
Except insoluble element state impurity contained in liquid aluminum isopropylate., it is thus achieved that ultra-pure liquid aluminum isopropylate.；
(3) hydrolyze, be aged and drying process: ultra-high purity isopropanol aluminum is slowly injected in hydrolysis ageing drying chamber, the most slowly
Inject high purity water and the hydrolyzed solution of isopropanol composition, issue raw hydrolysis in water-bath and stirring condition, obtain ultra-pure nanometer
Algeldrate and isopropanol water solution；Then, being aged in hydrolysis ageing drying chamber, be dried after ageing, liquid is different
Propanol becomes gaseous state isopropanol, condensed after become liquid anhydrous isopropanol and discharge, and ultra-pure nano-aluminum hydroxide is with solid-state
Powder type is stayed in hydrolysis ageing drying chamber body；
(4) calcine technology: ultra-pure nano-aluminum hydroxide powder is calcined, obtains Al2 O 3Powder；
(5) crushing packing technique: to Al2 O 3Powder pulverize after metering packing；
(6) tail gas treatment process: the isopropanol tail gas produced in step (1)～(3) is recycled by retracting device,
Reclaim after the liquid isopropanol obtained is dehydrated as the isopropanol raw material in described step (1).
In described step (3), described hydrolysis employing two-step hydrolysis technique:
The first step: the liquid high puring aluminium isopropoxide of metering is slowly put in hydrolysis ageing drying chamber, simultaneously in 60 DEG C of water-baths
It is slowly added to hydrolyzed solution while stirring, after reaction a period of time, steams water content less than 0.2 in 20mmHg, 60 DEG C of decompression distillations
Isopropanol, as the isopropanol raw material of synthesis technique in described step (1)；
Second step: disposably adding hydrolyzed solution in the product of distillation to first step distillation gained, reaction aging is after 24 hours,
20mmHg, 90 DEG C of decompressions steam the water content isopropanol more than 10%, for as the hydrolysis in the described first step
Hydrolyzed solution raw material.
In described step (1), the purity of described rafifinal bits is more than 99.99%, and described catalyst is mercuric chloride or aluminum chloride
Or aluminum isopropylate., described iron removing reagent is phenolphthalein or PAN or xylenol orange；Described desiliconizing agent is phenolphthalein or lanthanide oxide, described
The addition of catalyst is aluminum: catalyst=1: 0.01 ~ 0.05mol, and the addition of described iron removing reagent is aluminum: iron removing reagent=500:
1wt, the addition of described desiliconizing agent is aluminum: desiliconizing agent=100:1wt, and the heating-up temperature in the reactor of described step (1) is 84
～120 DEG C；In described step (1), the condensation temperature of condenser is 20～30 DEG C.
Described in described step (2), the vacuum in distillating still is 1 ~ 20mmHg, and temperature is 160 ~ 198 degrees Celsius；Described
Nano ceramics Membrane filtering machine is used for filtering out in liquid high puring aluminium isopropoxide contained insoluble element state Fe, Si, Cu impurity.
In described step (3), the high purity water in described hydrolyzed solution be resistivity be the high purity water of 15 ~ 18 megaohms, described water
Solve liquid also include hydrolyze auxiliary agent, in hydrolyzed solution the mass ratio of high purity water, isopropanol and hydrolysis auxiliary agent be 1: 1～8: 0.05～
0.5；Hydrolysis temperature is 50～110 DEG C, and hydrolysis time is 2 ~ 12h；
The ageing liquid of described aging crystallization is made up of solvent and ageing auxiliary agent, and solvent is the mixed liquor of water and below C4 alcohol, institute
Stating alcohol content in solvent is 1～50%wt；Ageing auxiliary agent is ammonium acetate, ammonium nitrate, acetic acid, ammonia, ammonium carbonate, carbamide, below C6
One or more in water solublity organic base, ageing auxiliary agent concentration in ageing liquid is 0.1～30%wt；Aluminium hydroxide is with old
Changing liquid mass ratio is 1: 3～30；Aging Temperature is 25～100 DEG C, and digestion time is 0.5～7 day；
Described baking temperature is 60～100 DEG C, drying time 2～12h；
In described step (4), the temperature of described calcining is 1180 DEG C-1250 DEG C, and calcination time is 5-6 hour.
The invention allows for a kind of ultra-pure nano aluminium oxide green syt industrialization device, including: synthetic reaction system
System (I): be used for carrying out synthetic reaction, obtain liquid aluminum isopropylate.；Distilation system (II): for described liquid isopropanol
Aluminum carries out distilation, obtains ultra-pure liquid aluminum isopropylate.；Hydrolysis drying system (III): be used for being hydrolyzed, be aged and doing
Dry, obtain ultra-pure aluminium hydrate powder；Calcination system (IV): for ultra-pure nano-aluminum hydroxide powder is calcined,
To Al2 O 3Powder；Broken package system (V): for Al 2 O 3Powder pulverize after metering packing；Isopropanol tail gas
Recovery system (VI): for collecting the isopropyl produced in described synthesis reaction system, distilation system and hydrolysis drying system
Alcohol tail gas, and it is transferred to described synthesis reaction system after being converted into liquid isopropanol.
Described synthesis reaction system (I) includes that isopropanol storage tank, isopropanol dehydration device, isopropanol measuring tank and synthesis are anti-
Answer tower；Described distilation system (II) includes distillating still, splice jug, distillation vacuum pump and nano ceramic membrane filter；Described
Hydrolysis drying system (III) includes aqueous isopropanol measuring tank, aluminum isopropylate. measuring tank, hydrolysis ageing drying chamber, anhydrous isopropyl alcohol
Storage tank, aqueous isopropanol storage tank and hydrolysis vacuum pump.
Described isopropanol exhaust gas recovery system includes isopropanol exhaust gas processing device and isopropanol tail gas air-introduced machine, described different
The air inlet of propanol exhaust gas processing device and the isopropanol exhaust port of described synthetic reaction tower, the tail of described distillation vacuum pump
The exhaust port of gas floss hole and described hydrolysis vacuum pump connects, and the outlet of described isopropanol exhaust gas processing device is with described
Isopropanol storage tank is connected；The outlet of described anhydrous isopropyl alcohol storage tank is connected with the import of described isopropanol measuring tank, described aqueous
The outlet of isopropanol storage tank is connected with the import of described aqueous isopropanol storage tank.
Described calcination system (IV) includes electricity push pedal calcining furnace and corundum body；Described broken package system (V) includes,
Corundum double-roll crusher, corundum airflow milling, bag filter and vacuum packing machine；Described synthetic reaction tower is anti-by the heating of bottom
The condenser answering still and top forms, and described reacting by heating still material is acid-resistant stainless steel, and described condenser is that glass tubulation is cold
Condenser.
Described one ultra-pure nano aluminium oxide green syt industrialization device, also includes: high purity water unit: be used for be
Hydrolysis ageing drying chamber in described hydrolysis drying system (III) prepares the high purity water in hydrolyzed solution；Self-controlling electrothermal hydrophone: be used for
Heating source is provided for described hydrolysis ageing drying chamber；Automatic control conductance hot oil furnace: for carrying for described synthetic reaction tower and distillating still
For heating source.
The present invention compared with prior art has the advantages that
(1) low cost: with cheap aluminium ingot as raw material, petrohol aluminum replaces directly using expensive aluminum isopropylate. preparation to receive
Rice aluminium oxide, reduces production cost；The a large amount of alcohol that will produce during reaction, rectification, separation etc., recycle, save former
Material, reduce further production cost
(2) low environmental load: aqueous phase, solvent phase, raw material all do not contain noxious substance；Solvent recovery is have employed in technical process
Technology, does not produce harmful gas, does not discharge harmful liquid, it is achieved the zero-emission of waste liquid in production process, is an environmental protection
Ultra-pure nano-oxide production technology.
Therefore, the present invention proposes ultra-pure nano aluminium oxide green synthesis method and industrialization device are possible not only to promote
The nanotechnology of China, shortens the nano material industry developed country such as China and Japan, German and U.S. and grinds at nano aluminium oxide
Study carefully and the gap in green synthesis techniques, and three-waste free pollution, it is truly realized cleaning production prepared by high purity nanometer alumina,
It it is the nano material production technology of " green ".The product of the present invention can be supplied and produce sapphire producer both at home and abroad, is used for giving birth to
Produce LED wafer, LED light fixture, high-performance ceramic etc., be possible not only to meet growing domestic and international market needs, moreover it is possible to promote
Enter China's fluorescent material, function ceramics, composite, moisture-sensitive sensor, integrated circuit pole plate, electricity-saving lamp and INFRARED ABSORPTION material
The development of the related industries such as material, has important social and economic significance.
Accompanying drawing explanation
Fig. 1 is the process chart of ultra-pure nano aluminium oxide green synthesis method that the present invention proposes；
Fig. 2 is the module diagram of ultra-pure nano aluminium oxide preparation technology equipment that the present invention proposes；
Fig. 3 is the connection diagram of ultra-pure nano aluminium oxide preparation technology equipment that the present invention proposes；
In Fig. 3: 1-isopropanol storage tank；2-isopropanol dehydration device；3-isopropanol measuring tank；4-synthetic reaction tower；5-distillating still；
6-splice jug；7-distills vacuum pump；8-hydrolysis ageing drying chamber；9-anhydrous isopropyl alcohol storage tank；10-aqueous isopropanol storage tank；11-
Hydrolysis vacuum pump；12-electricity push pedal calcining furnace；13-corundum double-roll crusher；14-corundum airflow milling；15-bag filter；16-
Bag filter air-introduced machine, 17-high purity water unit；18-automatic control water heater；19-aqueous isopropanol measuring tank；20-automatic control conductance
Hot oil furnace；21-isopropanol exhaust gas processing device；22-isopropanol tail gas air-introduced machine；23-aluminum isopropylate. delivery pump；24-ceramic membrane
Filter；25-aluminum isopropylate. storage tank；26-aluminum isopropylate. delivery pump；27-aluminum isopropylate. measuring tank；28-vacuum packing machine；29-
Oil-free screw compressor.
Detailed description of the invention
With specific embodiment, the present invention is described below in conjunction with the accompanying drawings again, but the summary of the invention of the present invention not only limits
Content in embodiment.
As it is shown in figure 1, the process chart of the ultra-pure nano aluminium oxide green synthesis method proposed for the present invention, this
Bright step of preparation process is:
(1) raw material prepares: buys isopropanol by GB GB7814-87, carries out processed with isopropanol dehydration device 2, will
High-purity aluminium ingot of buying by GB GB8178-87 (purity 99.99% and more than) is processed into aluminum bits.Automatic control conductance deep fat
Stove 20 adds full conduction oil, and opens heating system.
(2) synthesis: weigh 187.4kg aluminum bits (purity 99.99%, course of reaction loss 3%), add isopropyl
Aluminium alcoholates 45kg, isopropanol 310.5kg.Join the synthetic reaction tower 4 being made up of bottom reacting by heating still and upper condensator
In, adding catalyst, iron removing reagent, desiliconizing agent post-heating, temperature controls at 84-120 DEG C, isopropanol and aluminum generation synthetic reaction,
Generate gaseous state aluminum isopropylate.；Gaseous state aluminum isopropylate. enters condenser, after condensed device is cooled to liquid aluminum isopropylate., is back to anti-
Answering in still, the most ceaselessly evaporation-condensation-backflow, complete synthetic reaction, final aluminum bits and isopropanol generate liquid isopropyl completely
Aluminium alcoholates；Its chemical equation is:
2Al+6C 3 H 7OH=2Al (C3 H 7 O) 3 +3H 2↑
React through a few hours, observe liquid boiling in the reacting by heating still of synthetic reaction tower 4 bottom, reacting by heating still top
Analyzing in condenser blow-down pipe has no hydrogen to release.Through reaction after a while, depending on the consumption of isopropanol, constantly add isopropyl
Alcohol, addition is by isopropanol measuring tank 3 note amount.In course of reaction, always aluminum is excessive, controls reaction speed by adding isopropanol
Degree, when isopropanol accumulation be added to 1202kg time, argenteous aluminum bits almost without, illustrate that reaction comes into coda.The most
Adding 60kg isopropanol, make that reaction carries out is more complete.The isopropanol added amounts to 1260.2kg.Use up isopropanol
1202kg, remaining 60kg.Generate aluminum isopropylate. 6.67Kmol (1362.35kg).Synthetic reaction process symbiosis becomes 10.0Kmol
Hydrogen.
Wherein, described catalyst can be mercuric chloride or aluminum chloride or aluminum isopropylate., described iron removing reagent can be phenolphthalein or
PAN or xylenol orange；Described desiliconizing agent can be phenolphthalein or lanthanide oxide, and the addition of described catalyst is aluminum: catalyst
=1: 0.01 ~ 0.05mol, the addition of described iron removing reagent is Al: iron removing reagent=500:1 wt, and the addition of described desiliconizing agent is
Al: desiliconizing agent=100:1wt, the temperature of described condenser is 20～30 DEG C.
(3) distillation: 1362.35kg liquid aluminum isopropylate. is put in distillating still 5, heating evaporation isopropanol, temperature control
Make and steam the isopropanol in alumina gel at 98～120 DEG C, then evacuate distillating still 5 by distillation vacuum pump 7, work as vacuum
Degree reaches 10mm Hg post, and temperature reaches 160-198 DEG C, and aluminum isopropylate. colloidal sol starts distillation, condensed one-tenth white gels, puts
Enter splice jug 6.This process aluminum isopropylate. loss 1%, the liquid aluminum isopropylate. i.e. entering splice jug 6 is 1348kg,
6.60kmol。
Wherein, the vacuum in described distillating still 5 is 1 ~ 20mmHg, and temperature is 160 ~ 198 degrees Celsius.
(4) filter: the liquid high puring aluminium isopropoxide in splice jug 6 (160 DEG C) while hot is crossed nano ceramics Membrane filtering machine 24,
Filter the impurity such as insoluble element state Fe, Si, Cu contained by liquid high puring aluminium isopropoxide, it is thus achieved that ultra-high purity isopropanol aluminum, this process is different
Aluminum tripropoxide loss 1%, the ultra-pure liquid aluminum isopropylate. i.e. entering high puring aluminium isopropoxide storage tank 25 is 1334.5kg.
(5) hydrolyze, be aged, be dried: be slow after liquid ultra-high purity isopropanol aluminum is weighed by aluminum isopropylate. measuring tank 27
Slow play enters in hydrolysis ageing drying chamber 8, is slowly injected into high purity water, isopropanol, the hydrolyzed solution of hydrolysis auxiliary agent composition, in water-bath with stir
There is hydrolysis under the conditions of mixing, obtain ultra-pure nano-aluminum hydroxide and its reaction equation of isopropanol water solution is:
Al(C 3H 7O) 3 +3H2O=Al (OH) 3+3C 3H 7OH
Hydrolysis employing two step hydrolysis method: the first step, slowly puts into hydrolysis ageing drying chamber 8 by the liquid high puring aluminium isopropoxide of metering
In, in 60 DEG C of water-baths, it is slowly added to a certain amount of hydrolyzed solution (ultra-pure liquid aluminum isopropylate.: high purity water=1 while stirring simultaneously
~ 1.5) react, in hydrolyzed solution: containing high purity water 12%, containing isopropanol 88%, high purity water be resistivity be the height of 15 ~ 18 megaohms
Pure water, can be obtained after high purity water unit 17 by tap water, after reacting 4 hours, steams contain in 20mmHg, 60 DEG C of decompression distillations
The water yield isopropanol less than 0.2 enters anhydrous isopropyl alcohol storage tank 9, is transported to isopropanol measuring tank 3, as in synthetic reaction
The raw material of petrohol aluminum.
Second step, a certain amount of (the ultra-pure liquid isopropanol of disposable addition in the product of distillation of first step distillation gained
Aluminum: high purity water=1 ~ 1.5) hydrolyzed solution, in hydrolyzed solution: containing high purity water 12%, containing isopropanol 88% and a small amount of hydrolysis auxiliary agent, instead
After should completing, be aged 24 hours, 20mmHg, 60 DEG C decompression steam water content 12% isopropanol entrance aqueous isopropanol
Measuring tank 10, is transported to aqueous isopropanol storage tank 19, is used for as the isopropanol raw material in the hydrolyzed solution of aluminum isopropylate., after distillation
The product of gained is aluminium hydroxide.
The aluminum isopropylate. that this process enters in hydrolysis ageing drying chamber 8 is 1334.5kg.Hydrolysis ageing drying chamber 8 is by certainly
Control electric heater 18 heats.
After each one-step hydrolysis completes, hydrolysis ageing drying chamber 8 being heated to 80 ~ 99 DEG C, it is different that liquid isopropanol becomes gaseous state
Propanol, by vacuum system suction condenser system, becomes liquid isopropanol and discharges, and anhydrous isopropyl alcohol is used for the raw material of aluminum isopropylate.,
Aqueous isopropanol is used for hydrolyzing workshop section's hydrolyzed solution；And ultra-pure nano-aluminum hydroxide stays hydrolysis drying machine with solid powder form
In tank body.
Wherein, hydrolysis temperature can be 50～110 DEG C, and hydrolysis time is 2 ~ 12h；High purity water, isopropanol in hydrolyzed solution
With hydrolysis auxiliary agent quality can ratio for 1: 1～8: 0.05～0.5；The ageing liquid of described aging crystallization is by solvent and ageing
Auxiliary agent forms, and solvent is the mixed liquor of water and below C4 alcohol, and in described solvent, alcohol content is 1～50%wt；Ageing auxiliary agent is
One or more in ammonium acetate, ammonium nitrate, acetic acid, ammonia, ammonium carbonate, carbamide, below C6 water solublity organic base, ageing auxiliary agent exists
In ageing liquid, concentration is 0.1～30%wt；Aluminium hydroxide is 1: 3～30 with ageing liquid mass ratio；Aging Temperature be 25～
100 DEG C, digestion time is 0.5～7 day, and ultra-pure nano-aluminum hydroxide crystallite baking temperature is 60～100 DEG C, when being dried
Between 2～12h.
(6) calcining: loaded by dry ultra-pure nano-aluminum hydroxide powder in corundum crucible, forges in electricity pushed bat kiln
Burning, aluminium-hydroxide powder becomes Al2 O 3 Powder, its reaction equation is:
2Al(OH) 3=Al2O 3 +3H 2O
If γ-Al to be produced2O3, calcining heat is 800-950 DEG C, if α-Al to be produced2O3Calcining heat reaches
1150-1300℃.The A1 (OH) 3 of 6.60Kmol calcines to obtain the Al of 3.3Kmol2O3I.e. 336.46kg, year produce day be
300 days, annual production was 100.938 tons.
Wherein, α-Al to be produced2O3, the temperature of calcining is preferably 1180 DEG C-1250 DEG C, and calcination time is 5～6
Hour.
(7) pulverize, weigh, packaging: γ-aluminium oxide or α-aluminium oxide after calcining pass through corundum double-roll crusher
13 and corundum airflow milling 14 pulverize, by grading, put in storage by bag filter 15 and vacuum packing machine 28 weighing and bagging.This
Sample completes a production cycle, and what this circulation can go round and begin again goes on.
(8) isopropanol tail gas recycle: for reduce environmental pollution, reduce production cost, by with isopropanol tail gas air-introduced machine
The 22 isopropanol exhaust gas processing devices 21 connected reclaim distillation vacuum pump 7 and and the water that synthetic reaction tower 4 is connected with splice jug 6
Solve the isopropanol tail gas that the hydrolysis vacuum pump 11 that ageing drying chamber 8 connects is discharged, and obtain liquid isopropanol after processing, enter
Enter isopropanol storage tank 1, after isopropanol dehydration device 2, enter isopropanol measuring tank 3, as the isopropanol raw material of synthetic reaction,
Make tail gas qualified discharge.Isopropanol exhaust gas processing device 21 can be isopropanol tail gas NACF retracting device.
(9) finally to product A l2 O 3Powder body is tested: use ICP-OES, i.e. Plasma-Atomic Emission spectrum
Instrument, carries out impurities analysis to product, detects for a long time through domestic authority testing agency, and result shows Impurity Fe ＜
3ppm, Si ＜ 2ppm, Ca ＜ 1ppm, Na ＜ 1ppm, Mg ＜ 1ppm, Cr ＜ 1ppm, Al2 O 3Content >=
99.999%, reach ultra-pure standard.
One ultra-pure nano aluminium oxide green syt industrialization device that table 1 below provides for the present invention relates to equip number
Relation table between amount and industrialization volume of production.As can be seen from the table, the industrialization device that the present invention proposes, can be according to life
Yield increases the quantity of corresponding device, and extensibility is strong.
Table 1 ultra-pure nano aluminium oxide industrialization device catalog
As shown in Figures 2 and 3, the connection signal of industrialization device prepared by the ultra-pure nano aluminium oxide proposed for the present invention
Figure.The industrialization device of the present invention is mainly by synthesis reaction system I, distilation system II, hydrolysis drying system III, calcining system
System IV, crushing system V, isopropanol exhaust gas recovery system VI；Wherein, synthesis reaction system I is used for carrying out synthetic reaction, obtains
Liquid aluminum isopropylate.；Distilation system II, for described liquid aluminum isopropylate. is carried out distilation, obtains ultra-pure liquid
Aluminum isopropylate.；Hydrolysis drying system III: be used for being hydrolyzed, be aged and being dried, obtain ultra-pure aluminium hydrate powder；Calcination system
IV: for ultra-pure nano-aluminum hydroxide powder is calcined, obtain Al2 O 3Powder；Broken package system V: for right
Al 2 O 3Powder pulverize after metering packing；Isopropanol exhaust gas recovery system VI: be used for collecting described synthesis reaction system,
The isopropanol tail gas produced in distilation system and hydrolysis drying system, and it is transferred to described conjunction after being converted into liquid isopropanol
Become response system I as the isopropanol raw material of synthetic reaction.
Wherein, described synthesis reaction system I includes isopropanol storage tank 1, isopropanol dehydration device 2, isopropanol measuring tank 3 He
Synthetic reaction tower 4, described distilation system II includes distillating still 5, splice jug 6, distillation vacuum pump 7 and nano ceramics membrane filtration
Device 24；Described hydrolysis drying system III includes aqueous isopropanol measuring tank 19, aluminum isopropylate. measuring tank 27, hydrolysis ageing drying chamber
8, anhydrous isopropyl alcohol storage tank 9, aqueous isopropanol storage tank 10 and hydrolysis vacuum pump 11.
Wherein, described isopropanol exhaust gas recovery system VI includes isopropanol exhaust gas processing device 21 and isopropanol tail gas air inducing
Machine 22, the air inlet of described isopropanol exhaust gas processing device 21 and the isopropanol exhaust port of described synthetic reaction tower 4, described
The exhaust port of distillation vacuum pump 7 and the exhaust port of described hydrolysis vacuum pump 11 connect, at described isopropanol tail gas
The outlet of reason device is connected with described isopropanol storage tank 1；The outlet of described anhydrous isopropyl alcohol storage tank 9 and described isopropanol measuring tank
The import of 4 connects, and the outlet of described aqueous isopropanol storage tank 10 is connected with the import of described aqueous isopropanol storage tank 19.Wherein,
Isopropanol exhaust gas processing device 21 can be isopropanol tail gas activated carbon fiber retracting device.
Wherein, described calcination system IV includes electricity push pedal calcining furnace 12 and corundum body；Described broken package system VI wraps
Include corundum double-roll crusher 13, corundum airflow milling 14, bag filter 15 and vacuum packing machine 28, described synthetic reaction tower 4 by
The reacting by heating still of bottom and the condenser composition on top, described reacting by heating still material is acid-resistant stainless steel, described condenser
For glass pipe bundle condenser.
Wherein, described one ultra-pure nano aluminium oxide green syt industrialization device, also include: high purity water unit
17, self-controlling electrothermal hydrophone (18) and automatic control conductance hot oil furnace 20, high purity water unit 17 is for preparing for described hydrolysis drying system
High purity water in hydrolyzed solution；Self-controlling electrothermal hydrophone 18 is for providing heating source for described hydrolysis drying chamber；Automatic control conductance hot oil furnace
20 for providing heating source for described synthetic reaction tower 4 and distillating still 5.
Above in conjunction with accompanying drawing, embodiments of the invention are explained in detail, but the present invention is not limited to above-mentioned enforcement
Example, in the ken that those of ordinary skill in the art are possessed, it is also possible to make on the premise of without departing from present inventive concept
Go out various change.
Claims (10)
1. a ultra-pure nano aluminium oxide green synthesis method, it is characterised in that its processing step is:
(1) synthesis technique: by rafifinal bits and isopropanol, joins the reactor heated by bottom and upper condensator forms
In synthetic reaction tower, add catalyst, iron removing reagent, desiliconizing agent post-heating, isopropanol and aluminum generation synthetic reaction, generate gaseous state different
Aluminum tripropoxide；Gaseous state aluminum isopropylate. enters condenser, after condensed device is cooled to liquid aluminum isopropylate., is back to described reactor
In, the most ceaselessly evaporation-condensation-backflow, complete synthetic reaction, final aluminum bits and isopropanol generate liquid isopropanol completely
Aluminum；
(2) distilation technique: liquid aluminum isopropylate. is injected in distillating still and flash to aluminum isopropylate. steam, after entering splice jug
Become liquid high puring aluminium isopropoxide, then liquid high puring aluminium isopropoxide is crossed at a temperature of 160 DEG C nano ceramics Membrane filtering machine, filter
Except insoluble element state impurity contained in liquid aluminum isopropylate., it is thus achieved that ultra-pure liquid aluminum isopropylate.；
(3) hydrolyze, be aged and drying process: ultra-high purity isopropanol aluminum is slowly injected in hydrolysis ageing drying chamber, the most slowly
Inject high purity water and the hydrolyzed solution of isopropanol composition, issue raw hydrolysis in water-bath and stirring condition, obtain ultra-pure nanometer
Algeldrate and isopropanol water solution；Then, being aged in hydrolysis ageing drying chamber, be dried after ageing, liquid is different
Propanol becomes gaseous state isopropanol, condensed after become liquid anhydrous isopropanol and discharge, and ultra-pure nano-aluminum hydroxide is with solid-state
Powder type is stayed in hydrolysis ageing drying chamber body；
(4) calcine technology: ultra-pure nano-aluminum hydroxide powder is calcined, obtains Al2 O 3Powder；
(5) crushing packing technique: to Al2 O 3Powder pulverize after metering packing；
(6) tail gas treatment process: the isopropanol tail gas produced in step (1)～(3) is recycled by retracting device,
Reclaim after the liquid isopropanol obtained is dehydrated as the isopropanol raw material in described step (1).
One the most according to claim 1 ultra-pure nano aluminium oxide green synthesis method, it is characterised in that described step
(3) in, described hydrolysis employing two-step hydrolysis technique:
The first step: the liquid high puring aluminium isopropoxide of metering is slowly put in hydrolysis ageing drying chamber, simultaneously in 60 DEG C of water-baths
It is slowly added to hydrolyzed solution while stirring, after reaction a period of time, steams water content less than 0.2 in 20mmHg, 60 DEG C of decompression distillations
Isopropanol, as the isopropanol raw material of synthesis technique in described step (1)；
Second step: disposably adding hydrolyzed solution in the product of distillation to first step distillation gained, reaction aging is after 24 hours,
20mmHg, 90 DEG C of decompressions steam the water content isopropanol more than 10%, for as the hydrolysis in the described first step
Hydrolyzed solution raw material.
One the most according to claim 1 ultra-pure nano aluminium oxide green synthesis method, it is characterised in that described step
(1), in, the purity of described rafifinal bits is more than 99.99%, and described catalyst is mercuric chloride or aluminum chloride or aluminum isopropylate., described
Iron removing reagent is phenolphthalein or PAN or xylenol orange；Described desiliconizing agent is phenolphthalein or lanthanide oxide, and the addition of described catalyst is
Aluminum: catalyst=1: 0.01 ~ 0.05mol, the addition of described iron removing reagent is aluminum: iron removing reagent=500:1wt, described desiliconizing agent
Addition is aluminum: desiliconizing agent=100:1wt, and the heating-up temperature in the reactor of described step (1) is 84～120 DEG C；Described step
(1) in, the condensation temperature of condenser is 20～30 DEG C.
One the most according to claim 1 ultra-pure nano aluminium oxide green synthesis method, it is characterised in that described step
(2) vacuum in distillating still described in is 1 ~ 20mmHg, and temperature is 160 ~ 198 degrees Celsius；Described nano ceramics Membrane filtering machine
For filtering out contained insoluble element state Fe, Si, Cu impurity in liquid high puring aluminium isopropoxide.
One the most according to claim 1 ultra-pure nano aluminium oxide green synthesis method, it is characterised in that described step
(3) in, the high purity water in described hydrolyzed solution be resistivity be the high purity water of 15 ~ 18 megaohms, described hydrolyzed solution also includes that hydrolysis helps
Agent, in hydrolyzed solution, the mass ratio of high purity water, isopropanol and hydrolysis auxiliary agent is 1: 1～8: 0.05～0.5；Hydrolysis temperature is 50
～110 DEG C, hydrolysis time is 2 ~ 12h；
The ageing liquid of described aging crystallization is made up of solvent and ageing auxiliary agent, and solvent is the mixed liquor of water and below C4 alcohol, institute
Stating alcohol content in solvent is 1～50%wt；Ageing auxiliary agent is ammonium acetate, ammonium nitrate, acetic acid, ammonia, ammonium carbonate, carbamide, below C6
One or more in water solublity organic base, ageing auxiliary agent concentration in ageing liquid is 0.1～30%wt；Aluminium hydroxide is with old
Changing liquid mass ratio is 1: 3～30；Aging Temperature is 25～100 DEG C, and digestion time is 0.5～7 day；
Described baking temperature is 60～100 DEG C, drying time 2～12h；
In described step (4), the temperature of described calcining is 1180 DEG C-1250 DEG C, and calcination time is 5-6 hour.
6. a ultra-pure nano aluminium oxide green syt industrialization device, it is characterised in that including:
Synthesis reaction system (I): be used for carrying out synthetic reaction, obtain liquid aluminum isopropylate.；
Distilation system (II): for described liquid aluminum isopropylate. is carried out distilation, obtain ultra-pure liquid isopropanol
Aluminum；
Hydrolysis drying system (III): be used for being hydrolyzed, be aged and being dried, obtain ultra-pure aluminium hydrate powder；
Calcination system (IV): for ultra-pure nano-aluminum hydroxide powder is calcined, obtain Al2 O 3Powder；
Broken package system (V): for Al 2 O 3Powder pulverize after metering packing；
Isopropanol exhaust gas recovery system (VI): be used for collecting described synthesis reaction system, distilation system and hydrolysis and be dried system
The isopropanol tail gas produced in system, and it is transferred to described synthesis reaction system after being converted into liquid isopropanol.
One the most according to claim 6 ultra-pure nano aluminium oxide green syt industrialization device, it is characterised in that institute
State synthesis reaction system (I) and include that isopropanol storage tank (1), isopropanol dehydration device (2), isopropanol measuring tank (3) and synthesis are anti-
Answer tower (4),
Described distilation system (II) includes distillating still (5), splice jug (6), distillation vacuum pump (7) and nano ceramics membrane filtration
Device (24)；
Described hydrolysis drying system (III) includes aqueous isopropanol measuring tank (19), aluminum isopropylate. measuring tank (27), hydrolysis ageing
Drying chamber (8), anhydrous isopropyl alcohol storage tank (9), aqueous isopropanol storage tank (10) and hydrolysis vacuum pump (11).
One the most according to claim 7 ultra-pure nano aluminium oxide green syt industrialization device, it is characterised in that institute
State isopropanol exhaust gas recovery system and include isopropanol exhaust gas processing device (21) and isopropanol tail gas air-introduced machine (22), described isopropyl
The air inlet of alcohol exhaust gas processing device (21) and the isopropanol exhaust port of described synthetic reaction tower (4), described distillation vacuum
The exhaust port of pump (7) and the exhaust port of described hydrolysis vacuum pump (11) connect, and described isopropanol vent gas treatment fills
The outlet put is connected with described isopropanol storage tank (1)；
The outlet of described anhydrous isopropyl alcohol storage tank (9) is connected with the import of described isopropanol measuring tank (4), described aqueous isopropanol
The outlet of storage tank (10) is connected with the import of described aqueous isopropanol storage tank (19).
One the most according to claim 7 ultra-pure nano aluminium oxide green syt industrialization device, it is characterised in that institute
State calcination system and include electricity push pedal calcining furnace (12) and corundum body；
Described broken package system includes, corundum double-roll crusher (13), corundum airflow milling (14), bag filter (15) and true
Empty package machine (28)；
Described synthetic reaction tower (4) is made up of the reacting by heating still of bottom and the condenser on top, described reacting by heating still material
For acid-resistant stainless steel, described condenser is glass pipe bundle condenser.
One the most according to claim 7 ultra-pure nano aluminium oxide green syt industrialization device, it is characterised in that
Also include:
High purity water unit (17): prepare hydrolyzed solution for being aged drying chamber (8) for the hydrolysis in described hydrolysis drying system (III)
In high purity water；
Self-controlling electrothermal hydrophone (18): for providing heating source for described hydrolysis ageing drying chamber (8)；
Automatic control conductance hot oil furnace (20): for providing heating source for described synthetic reaction tower (4) and distillating still (5).
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| CN111841246A (en) * | 2020-07-09 | 2020-10-30 | 大连理工大学 | Method for treating tail gas in process for preparing high-purity pseudo-boehmite |
| CN112250452A (en) * | 2020-09-25 | 2021-01-22 | 新疆众和股份有限公司 | Alumina water-based coating material, preparation method thereof and crucible coating method |
| CN113149050A (en) * | 2021-04-13 | 2021-07-23 | 新疆众和股份有限公司 | Method for treating solid waste in high-purity alcohol aluminum salt industry |
| CN115490250A (en) * | 2022-10-24 | 2022-12-20 | 河北铭万精细化工有限公司 | Industrial production process of high-purity nano aluminum oxide |
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