CN105218446B - A kind of process for preparing pure 8 oxyquinoline barium - Google Patents
A kind of process for preparing pure 8 oxyquinoline barium Download PDFInfo
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- CN105218446B CN105218446B CN201510810195.0A CN201510810195A CN105218446B CN 105218446 B CN105218446 B CN 105218446B CN 201510810195 A CN201510810195 A CN 201510810195A CN 105218446 B CN105218446 B CN 105218446B
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- barium
- hydroxyquinoline
- reaction
- oxyquinoline
- room temperature
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
A kind of process for preparing pure 8 oxyquinoline barium of the present invention, is barium monoxide according to mol ratio using barium monoxide and 8 oxyquinolines as reactant:8 oxyquinoline=1:2, reaction raw materials barium monoxide and 8 oxyquinolines are added in ceramic grinder, grind the min of 30 min~40 at room temperature.Grinding is finished, and reaction mass is transferred in reactor, is passed through nitrogen N2Protection, it is warming up to the min of 130 DEG C~150 DEG C min of insulation reaction 90~120.Reaction finishes, and is cooled to room temperature, obtains 8 oxyquinoline barium products of yellow green, its purity is 98.5%~99.5%, yield is 96%~98%.The present invention has green, and raw material availability is high, and product purity is high, high income, the advantages such as production cost is low.
Description
Technical field
The present invention relates to a kind of process for preparing pure 8-hydroxyquinoline barium, more particularly to one kind with barium monoxide and 8-
Oxyquinoline is raw material, the method for preparing 8-hydroxyquinoline barium using solid-phase grinding-hot melt reaction method.The present invention particularly belongs to gold
Belong to organic coordination compound preparing technical field.
Background technology
After Chen Qingyun has found that 8-hydroxyquinoline aluminium has splendid luminescent properties, metallic element and 8-hydroxyquinoline and
The complex of its derivatives reaction generation turns into the study hotspot of luminous organic material.People are typically by selecting different metals
Element introduces functional group to improve luminescent properties on quinoline ring.In addition to aluminum, study at present it is more be zinc,
The 8-hydroxyquinoline class complex of the heavy metal elements such as copper.Although the 8-hydroxyquinoline class complex of the heavy metal elements such as zinc, copper
Luminescent properties it is fine, but the problems such as big for environment pollution be present.At present, the vision of metallic element is selected, is begun to transfer to
The metallic element that effect on environment is small, toxicity is low.Therefore, to the 8-hydroxyquinoline class complex of alkali earth metal is related grinds
Study carefully and start to be paid close attention to by professional person.
As the 8-hydroxyquinoline complex of other alkali earth metals, the preparation research of 8-hydroxyquinoline barium rarely has report
Road.It is Ribeiro in 2001 et al. in periodical to prepare the representational method of 8-hydroxyquinoline derivative Barium complex
“Journal of Thermal Analysis and Calorimetry" technical method disclosed in the 638th of volume 64：With hydration
Barium nitrate and 8-hydroxyquinoline derivative are reaction raw materials, and the acetone of the aqueous solution of barium nitrate and 8-hydroxyquinoline derivative is molten
Heating stirring reacts 60 min after liquid mixing, and the pH value that reaction solution is adjusted with concentrated ammonia liquor is 9.Reaction finishes, filtering, weak aqua ammonia
Wash unreacted compounding ingredient（8-hydroxyquinoline）, 60 DEG C of dryings, the Barium complex of 8-hydroxyquinoline derivative is obtained after cooling.
The existing method for preparing 8-hydroxyquinoline barium is also Traditional liquid phase method.In fact, the preparation method of 8-hydroxyquinoline barium and 8- hydroxyls
The preparation method of base quinoline Barium complex is similar.It is well known that Traditional liquid phase method generally existing technological process compared with
Length, waste liquor contamination are big（Salt-containing organic wastewater）, product yield it is low（Usually 60%~70%）, production cost it is high（8-hydroxyquinoline
Need excess）The shortcomings of.
The purity of luminescent material has a major impact to the characteristics of luminescence.Only purity is higher than 95% 8-hydroxyquinoline metalloid
Complex, it just can serve as luminescent material.How the shortcomings of liquid phase method are overcome, and directly preparing purity can be without higher than 95%
Purifying can be used as the 8-hydroxyquinoline barium of luminous organic material, be currently to need one of technical barrier for being captured.
The content of the invention
The purpose of the present invention is to prepare 8-hydroxyquinoline barium for Traditional liquid phase method to have that long flow path, waste liquor contamination be big, production
The shortcomings of product yield is low, production cost is high, proposes that a kind of short flow, production cost are low, green degree is high and prepare pure 8-
The new method of oxyquinoline barium.
The present invention chemical principle be：
BaO+ 2C9H6NOH = Ba(C9H6NO)2+ H2O
A kind of process for preparing pure 8-hydroxyquinoline barium of the present invention, using barium monoxide and 8-hydroxyquinoline as raw material, is pressed
It is barium monoxide according to mol ratio:8-hydroxyquinoline=1:2, reaction raw materials barium monoxide and 8-hydroxyquinoline are added in ceramic grinder,
The min of 30min~40 is ground at room temperature；Grinding is finished, and reaction mass is transferred in reactor, is passed through nitrogen N2Protection, heating
To the min of 130 DEG C~150 DEG C min of insulation reaction 90~120；Reaction finishes, and is cooled to room temperature, obtains the 8- hydroxyls of yellow green
Quinoline barium product, its purity is 98.5%~99.5%, yield is 96%~98%.
It is an advantage of the invention that：8-hydroxyquinoline barium is prepared using solid-phase grinding-hot melt reaction method, reactant and product
Toxicity is relatively low, high without discharging of waste liquid, reactant atom utilization, and technological process is easy, green；Reactant did not needed
Amount, the utilization rate of raw material are high；The purity of product 8-hydroxyquinoline barium is high, high income；The production cost of 8-hydroxyquinoline barium is low etc..
Embodiment
A kind of process for preparing pure 8-hydroxyquinoline barium of the present invention is made with reference to specific embodiment into
One step describes.
Embodiment 1：
It is barium monoxide according to mol ratio:8-hydroxyquinoline=1:2, by 100.00kg barium monoxide and 189.35 kg 8- hydroxyls
The reaction raw materials of quinoline enter in ceramic grinder, grind 35 min at room temperature；Grinding is finished, and reaction mass is transferred into reactor
In, it is passed through nitrogen N2Protection, is warming up to 140 DEG C of min of insulation reaction 105；Reaction finishes, and is cooled to room temperature, obtains yellow green
8-hydroxyquinoline barium product, its purity is 99.5%, yield 97%.
Embodiment 2：
It is barium monoxide according to mol ratio:8-hydroxyquinoline=1:2, by 100.00 kg barium monoxide and 189.35 kg 8- hydroxyls
The reaction raw materials of base quinoline enter in ceramic grinder, grind 30 min at room temperature；Grinding is finished, and reaction mass is transferred into reaction
In device, nitrogen N is passed through2Protection, is warming up to 150 DEG C of min of insulation reaction 90；Reaction finishes, and is cooled to room temperature, obtains yellow green
8-hydroxyquinoline barium product, its purity is 99.0%, yield 96%.
Embodiment 3：
It is barium monoxide according to mol ratio:8-hydroxyquinoline=1:2, by 100.00 kg barium monoxide and 189.35 kg 8- hydroxyls
The reaction raw materials of base quinoline enter in ceramic grinder, grind 40 min at room temperature；Grinding is finished, and reaction mass is transferred into reaction
In device, nitrogen N is passed through2Protection, is warming up to 130 DEG C of min of insulation reaction 120；Reaction finishes, and is cooled to room temperature, obtains yellow green
8-hydroxyquinoline barium product, its purity is 98.5%, yield 98%.
Claims (1)
- A kind of 1. process for preparing pure 8-hydroxyquinoline barium, it is characterised in that：Described process is with barium monoxide and 8- Oxyquinoline is raw material, is barium monoxide according to mol ratio:8-hydroxyquinoline=1:2, by reaction raw materials barium monoxide and 8-hydroxyquinoline Add in ceramic grinder, grind the min of 30 min~40 at room temperature；Grinding is finished, and reaction mass is transferred in reactor, It is passed through nitrogen N2Protection, it is warming up to the min of 130 DEG C~150 DEG C min of insulation reaction 90~120；Reaction finishes, and is cooled to room temperature, The 8-hydroxyquinoline barium product of yellow green is obtained, its purity is 98.5%~99.5%, yield is 96%~98%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510810195.0A CN105218446B (en) | 2015-11-23 | 2015-11-23 | A kind of process for preparing pure 8 oxyquinoline barium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510810195.0A CN105218446B (en) | 2015-11-23 | 2015-11-23 | A kind of process for preparing pure 8 oxyquinoline barium |
Publications (2)
| Publication Number | Publication Date |
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| CN105218446A CN105218446A (en) | 2016-01-06 |
| CN105218446B true CN105218446B (en) | 2018-01-16 |
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| CN201510810195.0A Expired - Fee Related CN105218446B (en) | 2015-11-23 | 2015-11-23 | A kind of process for preparing pure 8 oxyquinoline barium |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2015
- 2015-11-23 CN CN201510810195.0A patent/CN105218446B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (3)
| Title |
|---|
| Mixed Ligand Calcium Complexes of Azo Compounds;T. V. R. K. Rao et al.;《J. Inst. Chemists(India)》;19991231;第71卷(第2期);64 * |
| Photoluminescence of bis(8-hydroxyquinoline) zinc (Znq2) and magnesium (Mgq2);Taiju Tsuboi et al.;《Cent. Eur. J. Phys.》;20121231;第10卷(第2期);524-528 * |
| RN 869649-63-8 REGISTRY;-;《STN REGISTRY》;20051209 * |
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| CN105218446A (en) | 2016-01-06 |
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