CN104151239B - A kind of synthetic method of pure oxine aluminium - Google Patents
A kind of synthetic method of pure oxine aluminium Download PDFInfo
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- CN104151239B CN104151239B CN201410366875.3A CN201410366875A CN104151239B CN 104151239 B CN104151239 B CN 104151239B CN 201410366875 A CN201410366875 A CN 201410366875A CN 104151239 B CN104151239 B CN 104151239B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D215/00—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems
- C07D215/02—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom
- C07D215/16—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D215/20—Oxygen atoms
- C07D215/24—Oxygen atoms attached in position 8
- C07D215/26—Alcohols; Ethers thereof
- C07D215/30—Metal salts; Chelates
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The synthetic method of a kind of pure oxine aluminium of the present invention, with oxine and al formate for raw material, specifically comprises three steps.The first step adds materials: according to oxine: the mol ratio of al formate=3:1, is alternately added in ball grinder by reaction raw materials; Mill ball is agate ball, and mill ball and quality of material are than being 10:1 ~ 20:1.Second step ball-milling reaction: ball grinder vacuumizes, after vacuum tightness is less than 0.1Pa, stops bleeding, and starts ball milling; Drum's speed of rotation is 100r/min ~ 200r/min, and Ball-milling Time is 1h ~ 2h, obtains yellow product.3rd step vacuum-drying: second step gained yellow product is placed in Vacuumdrier, at 50 DEG C, vacuum-drying 2 h, obtains the oxine aluminium that purity is 97% ~ 99%.The present invention has the advantages such as productive rate is high, non-wastewater discharge, technical process is short, production cost is low.
Description
Technical field
The present invention relates to a kind of synthetic method of pure oxine aluminium, particularly relate to a kind of method taking al formate as main raw material, solid phase method and directly synthesize pure oxine aluminium.
Background technology
Oxine aluminium is a kind of ideal green luminescent material, has the good characteristics of luminescence, film-forming properties and thermostability, is widely used in organic electroluminescence device.But, the oxine aluminium that purity is greater than 95%, could be used as luminous organic material.At present, the method for industrialization synthesis oxine aluminium is liquid chemical precipitation method.Reaction raw materials is oxine and inorganic aluminate, the water-soluble aluminum salt such as such as Tai-Ace S 150, aluminum chloride, aluminum nitrate.General synthesis program is: first, by water-soluble for aluminium salt, oxine is dissolved in organic solvent, such as dehydrated alcohol etc.; Then, the organic solvent solution of oxine is added drop-wise in the aqueous solution of aluminium salt under certain condition; Finally, react complete, suction filtration, washing, drying.In the reaction system of various liquid chemical precipitation method synthesis oxine aluminium, modal liquid-phase system is water-ethanol system.Due to the acting in conjunction of oxygen in reaction system and water, and cause the side reactions such as oxine aluminium polymerization reaction take place, the oxine aluminium purity low (being generally 75% ~ 80%) causing liquid chemical precipitation method to be synthesized, productive rate are low.As a result, liquid chemical precipitation method directly can not synthesize the oxine aluminium of purity on 95%.Therefore, subliming method or column chromatography must be adopted repeatedly to purify to the oxine aluminium that liquid chemical precipitation method is synthesized, could obtain purity higher than 95% oxine aluminium to meet the requirement of luminescent material.But, subliming method or column chromatography purification process quite complicated, cannot produce in enormous quantities.And, in order to improve productive rate, usually make precipitation agent oxine greatly excessive.It can thus be appreciated that the synthetic method of the pure oxine aluminium of existing liquid chemical precipitation method, due to factors such as productive rate are low, flow process is complicated, industrial scale is little, must cause production cost high.Therefore, the method for existing industrialization synthesis oxine aluminium, not only production cost is high, and discharge contains the waste water of oxine and organic solvent.
Summary of the invention
There is flow process complexity, high, the heavy-polluted shortcoming of production cost in the method that the object of the invention is for existing industrialization synthesis oxine aluminium, proposes the novel method that a kind of short flow, production cost are low, pollute little synthesis oxine aluminium.
The present invention does not adopt liquid-phase reaction system, but adopts vacuum solid-phase reaction system.The detrimentally affect of water to synthesis oxine aluminium is eliminated by solid state reaction; The detrimentally affect of oxygen to synthesis oxine aluminium is eliminated by vacuumizing.Owing to eliminating the side reaction of water and oxygen initiation, the oxine aluminium purity of therefore synthesizing is high, and purity directly can reach 97% ~ 99%.Eliminate repeatedly purification operations complicated in liquid chemical precipitation method, can production cost be reduced.The present invention is by mechanical force strengthening reaction, and it is excessive that reaction raw materials oxine does not need, and can reduce production cost.Synthesis flow is brief, is easy to the pure oxine aluminium that extensive direct production purity meets luminescent material requirement, can reduces production cost.Solid-phase reaction system, neither uses water, and also not with an organic solvent, non-wastewater discharge, not only can protection of the environment, and can reduce production cost.
Reaction principle of the present invention is:
Al(HCOO)
3 + 3 C
9H
6NOH = Al(C
9H
6NO)
3+ HCOOH
The synthetic method of a kind of pure oxine aluminium of the present invention, adopts vacuum, solid-phase reaction system, with oxine and al formate for the pure oxine aluminium of Material synthesis, realizes especially by following steps:
The first step, adds materials
Be oxine according to mol ratio: al formate=3:1, alternately adds reaction raw materials in ball grinder; Mill ball is agate ball, and mill ball and quality of material are than being 10:1 ~ 20:1.
Second step, ball-milling reaction
Ball grinder vacuumizes, and after vacuum tightness is less than 0.1 Pa, stops bleeding, and starts ball milling; Drum's speed of rotation is 100 r/min ~ 200 r/min, and Ball-milling Time is 1 h ~ 2 h, obtains yellow product.
3rd step, vacuum-drying
Second step gained yellow product is placed in Vacuumdrier, and at 50 DEG C, vacuum-drying 2 h, obtains the oxine aluminium that purity is 97% ~ 99%.
Advantage of the present invention is: 1) non-wastewater discharge, protection of the environment.2) it is excessive that the reaction raw materials oxine that price is higher does not need.3) synthesis technique flow process is short.4) productive rate of oxine aluminium is high.5) production cost is low.6) during vacuum-drying, can reclaim formic acid, the utilising efficiency of reaction raw materials is high.
Embodiment
Be further described below in conjunction with the synthetic method of specific embodiment to a kind of pure oxine aluminium of the present invention.
embodiment 1:
The first step, adds materials
Be oxine according to mol ratio: al formate=3:1, alternately adds in 100 L ball grinders by reaction raw materials, oxine amounts to and adds 6.438 kg, and al formate amounts to and adds 2.395 kg.Mill ball is agate ball, and mill ball and quality of material are than being 15:1, and the quality of agate ball is 132.5 kg.
Second step, ball-milling reaction
Ball grinder vacuumizes, and after vacuum tightness is less than 0.1 Pa, stops bleeding, and starts ball milling; Drum's speed of rotation is 150 r/min, and Ball-milling Time is 1.5 h, obtains yellow product.
3rd step, vacuum-drying
Second step gained yellow product is placed in Vacuumdrier, and at 50 DEG C, vacuum-drying 2 h, obtains the oxine aluminium that purity is 98%.Vacuumize expellant gas and contain formic acid, adopt condensation method to reclaim formic acid.
embodiment 2:
The first step, adds materials
Be oxine according to mol ratio: al formate=3:1, alternately adds in 100 L ball grinders by reaction raw materials, oxine amounts to and adds 9.657 kg, and al formate amounts to and adds 3.593 kg.Mill ball is agate ball, and mill ball and quality of material are than being 10:1, and the quality of agate ball is 132.5 kg.
Second step, ball-milling reaction
Ball grinder vacuumizes, and after vacuum tightness is less than 0.1 Pa, stops bleeding, and starts ball milling; Drum's speed of rotation is 200 r/min, and Ball-milling Time is 1 h, obtains yellow product.
3rd step, vacuum-drying
Second step gained yellow product is placed in Vacuumdrier, and at 50 DEG C, vacuum-drying 2 h, obtains the oxine aluminium that purity is 97%.Vacuumize expellant gas and contain formic acid, adopt condensation method to reclaim formic acid.
embodiment 3:
The first step, adds materials
Be oxine according to mol ratio: al formate=3:1, alternately adds in 100 L ball grinders by reaction raw materials, oxine amounts to and adds 4.828 kg, and al formate amounts to and adds 1.797 kg.Mill ball is agate ball, and mill ball and quality of material are than being 20:1, and the quality of agate ball is 132.5 kg.
Second step, ball-milling reaction
Ball grinder vacuumizes, and after vacuum tightness is less than 0.1 Pa, stops bleeding, and starts ball milling; Drum's speed of rotation is 100 r/min, and Ball-milling Time is 2 h, obtains yellow product.
3rd step, vacuum-drying
Second step gained yellow product is placed in Vacuumdrier, and at 50 DEG C, vacuum-drying 2 h, obtains the oxine aluminium that purity is 99%.Vacuumize expellant gas and contain formic acid, adopt condensation method to reclaim formic acid.
Claims (1)
1. a synthetic method for pure oxine aluminium, is characterized in that: described synthetic method adopts vacuum, solid-phase reaction system, with oxine and al formate for the pure oxine aluminium of Material synthesis, realizes especially by following steps:
The first step, adds materials
According to oxine: the mol ratio of al formate=3:1, reaction raw materials is alternately added in ball grinder; Mill ball is agate ball, and mill ball and quality of material are than being 10:1 ~ 20:1;
Second step, ball-milling reaction
Ball grinder vacuumizes, and after vacuum tightness is less than 0.1 Pa, stops bleeding, and starts ball milling; Drum's speed of rotation is 100 r/min ~ 200 r/min, and Ball-milling Time is 1 h ~ 2 h, obtains yellow product;
3rd step, vacuum-drying
Second step gained yellow product is placed in Vacuumdrier, and at 50 DEG C, vacuum-drying 2 h, obtains the oxine aluminium that purity is 97% ~ 99%.
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| CN104151239B true CN104151239B (en) | 2015-10-21 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104649970A (en) * | 2015-02-09 | 2015-05-27 | 南昌航空大学 | Method for directly synthesizing organic luminous material, namely 8-hydroxyquinoline zinc |
| CN104744362A (en) * | 2015-04-08 | 2015-07-01 | 南昌航空大学 | Method for directly synthesizing pure copper 8-hydroxyquinoline |
| CN105237475B (en) * | 2015-11-23 | 2018-01-16 | 南昌航空大学 | A kind of green synthesis method of 8 oxyquinoline strontium |
| CN105348191B (en) * | 2015-11-30 | 2018-01-16 | 南昌航空大学 | A kind of method for directly preparing pure 8 oxyquinoline calcium |
| CN105622504B (en) * | 2015-12-26 | 2018-04-06 | 南昌航空大学 | A kind of green method for preparing the oxyquinoline barium of luminescent material 8 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1212261A (en) * | 1998-04-08 | 1999-03-31 | 新疆大学 | Method for preparing nanometre material by solid phase chemical reaction |
| CN103145614A (en) * | 2013-03-11 | 2013-06-12 | 新疆大学 | Method for preparing 8-hydroxyquinoline magnesium nano sheet by room-temperature solid-state chemical reaction |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1212261A (en) * | 1998-04-08 | 1999-03-31 | 新疆大学 | Method for preparing nanometre material by solid phase chemical reaction |
| CN103145614A (en) * | 2013-03-11 | 2013-06-12 | 新疆大学 | Method for preparing 8-hydroxyquinoline magnesium nano sheet by room-temperature solid-state chemical reaction |
Non-Patent Citations (3)
| Title |
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| 8-羟基喹啉铝晶体的制备与表征;陈杰等;《湖北汽车工业学院学报》;20100630;第24卷(第2期);第51-53，69页 * |
| 贾梦鑫等.8-羟基喹啉铝的制备与应用的研究进展.《广州化工》.2013,第41卷(第23期),第26-27,30页. * |
| 高纯8-羟基喹啉铝的简便合成方法;朱凌健等;《化学试剂》;20040630;第26卷(第6期);第369-370页 * |
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