CN102153570A - Quick synthesis method of reverse-2-(2-hydroxy styryl)-8-oxyquinoline zinc - Google Patents
Quick synthesis method of reverse-2-(2-hydroxy styryl)-8-oxyquinoline zinc Download PDFInfo
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Abstract
The invention relates to a synthesis method of reverse-2-(2-hydroxy styryl)-8-oxyquinoline zinc. In the method, organic and inorganic and solvent materials are used and a two-step synthesis method is adopted to first synthesize reverse-2-(2-acetoxyl group styryl)-8-acetoxyl group quinoline and then directly synthesize reverse-2-(2-hydroxy styryl)-8- hydroxyquinoline zinc by ester exchange reaction. The product is yellow powder being kelly; the color coordinate is: X is equal to 0.4312 and Y is equal to 0.4861. The purity is good up to 99.1%, the light emission performance is excellent, and the yield is as high as 91.7%. The synthesis method is advanced in process, quick and simple with two steps of synthesis, reasonable in mixing rate of all chemical substances, and accurate in process parameters, being a method for synthesizing materials with kelly light by using organic and inorganic and solvent substances.
Description
Technical field
The present invention relates to a kind of anti--fast synthesis method of 2-(2-hydroxystyrene based)-oxine zinc, belong to the preparation of electroluminescent organic material and the technical field of application.
Background technology
Since the U.S. C.W.Tang of Kadak company reported first in 1987 oxine aluminium as electroluminescent organic material since, be that the research of the organometallic complex of part becomes the emphasis that people pay close attention to always with the oxine; For improving the present situation that the oxine organometallic complex is insoluble in organic solvent, can carry out structural modification to the oxine part, mainly 2 at the quinoline ring introduce big conjugation substituting group, increase the rigid structure of oxine ring, HOMO and lumo energy are poor in the change molecular orbital(MO), obtain the good organo-metallic fluorescent material of solvability of different emission wavelengths; Introduce the big conjugation substituting group of o-hydroxy vinyl, also can obtain the better organo-metallic fluorescent material of solvability for 2 at the quinoline ring with the metallic zinc ionic reaction; Conventional method is synthetic by four steps: generate the product that contains acetoxyl group by 2-methyl-oxine and aromatic aldehyde reaction earlier; Form salt with the concentrated hydrochloric acid reaction; Form the hydroxyl part with the triethylamine reaction; Hydroxyl part and metal ion reaction obtain the target end product.
At present, the synthetic drawbacks such as complex steps, purification is complicated, production yield rate is low that exist of this type of material are greatly limited industrial applications.
Summary of the invention
Goal of the invention
The objective of the invention is at disadvantages of background technology; with 2-methyl-oxine, salicylic aldehyde, zinc acetate and diacetyl oxide is raw material; adopt two-step synthesis synthesizing yellow under electrically heated, magnetic agitation, water cycle condensation, oil bath state, nitrogen protection anti--2-(2-hydroxystyrene based)-oxine zinc; make the organic electroluminescence material of preparation jaundice green glow more rapid and simple, to increase substantially product purity and yield.
Technical scheme
The chemical substance material that the present invention uses is: 2-methyl-oxine, zinc acetate, salicylic aldehyde, ethanol, diacetyl oxide, ethyl acetate, triethylamine, deionized water, oil bath oil, nitrogen, its combination consumption is as follows: with gram, milliliter is measure unit
2-methyl-oxine: C
10H
9ON 3.58g ± 0.001g
Zinc acetate: (CH
3COO)
2Zn2H
2O 1.09g ± 0.001g
Salicylic aldehyde: C
7H
6O
22.76g ± 0.001g
Ethanol: C
2H
6O 1000ml ± 10ml
Diacetyl oxide: C
4H
6O
3100ml ± 2ml
Ethyl acetate: C
4H
8O
2200ml ± 5ml
Triethylamine: C
6H
15N 50ml ± 1ml
Deionized water: H
2O 3000ml ± 50ml
Nitrogen: N
220000cm
3± 100cm
3
Oil bath oil: 500ml ± 50ml
Fast synthesis method is as follows:
(1) selected chemical substance material
To carry out selectedly to preparing required chemical substance material, and carry out quality purity control:
2-methyl-oxine: solid-state solid 99.9%
Zinc acetate: solid-state solid 99.8%
Salicylic aldehyde: liquid liquid 99.0%
Ethanol: liquid liquid 99.9%
Diacetyl oxide: liquid liquid 99.9%
Ethyl acetate: liquid liquid 99.9%
Triethylamine: liquid liquid 99.9%
Deionized water: liquid liquid 99.9%
Nitrogen: gaseous state gas 99.8%
Oil bath oil: liquid liquid 90%
(2) anti-synthetic-2-(2-acetoxy-styrene base)-8-acetoxyl group quinoline
1. synthesize in there-necked flask and carry out, there-necked flask is placed on the oil bath cylinder, the oil bath cylinder is placed on the electric heating agitator, on there-necked flask, set gradually nitrogen tube, addition funnel, water cycle prolong from left to right;
Add oil bath oil 800ml in the oil bath cylinder, oil bath oil floods 9/10 of there-necked flask volume;
2. take by weighing salicylic aldehyde 2.76g ± 0.001g;
Take by weighing 2-methyl-oxine 3.58g ± 0.001g;
Take by weighing diacetyl oxide 70ml ± 0.1ml;
Add in the there-necked flask by addition funnel then;
3. open the electric heating agitator, temperature rises to 130 ℃ ± 2 ℃ by 25 ℃, 8 ℃/min of heat-up rate, and stir;
Open nitrogen tube, to there-necked flask input nitrogen, nitrogen input speed 22cm
3/ min;
Open the water cycle prolong, carry out the water cycle condensation;
Limit heating, limit stirring, limit water cycle condensation, limit input nitrogen, time 2400min fully dissolves the interior chemical substance of there-necked flask;
Become: 2-methyl-oxine+salicylic aldehyde+diacetyl oxide ternary mixing solutions;
In synthesis of ternary mixing solutions process, chemical reaction will take place, reaction formula is as follows:
In the formula: O: oxygen H: hydrogen
C: carbon H
3C: methyl
N: nitrogen OH: hydroxyl
4. after reaction finishes, close the electric heating agitator, the water cycle prolong is cooled to 25 ℃ with there-necked flask under nitrogen protection;
5. mixture of ice and water extraction
The preparation mixture of ice and water:
100ml places beaker with deionized water, places refrigerator and cooled to freeze then, makes it form ice cube under-10 ℃;
Add deionized water 100ml in beaker, mix stirring with ice cube, become: mixture of ice and water;
The ternary mixing solutions is added in the beaker, and stir 720min, become: the yellow tertiary mixture aqueous solution with agitator;
6. suction filtration
The tertiary mixture aqueous solution is placed B on the filter flask, carry out suction filtration with two layers of fast qualitative filter paper, retain the product filter cake on the filter paper, and collect, filtrate places filter flask to discard;
7. the washing, suction filtration
The product filter cake is placed beaker, add deionized water 100ml, agitator treating 5min;
Place the B on the filter flask then, carry out suction filtration with two layers of fast qualitative filter paper, retain the product filter cake on the filter paper, filtrate is evacuated in the filter flask and discards;
Washing, suction filtration repeat 5 times;
8. vacuum-drying
The product filter cake is placed quartz boat, place vacuum drying oven to carry out drying then, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 18Pa, time of drying, 60min became after the drying: buff powder;
9. recrystallization is purified
Buff powder is placed another there-necked flask, there-necked flask is placed on the oil bath cylinder, the oil bath cylinder is placed on the electric heating agitator, in there-necked flask, add ethyl acetate 30ml then, turn on agitator, 70 ℃ ± 2 ℃ of Heating temperatures, and carry out the water cycle condensation, heated and stirred 30min becomes: mixing solutions;
While hot mixing solutions is placed on the filter funnel, filter with two layers of fast qualitative filter paper, solution places filter flask;
Filtrate is still aging 120min in filter flask, slowly separates out white crystal;
10. vacuum-drying
Solution is placed beaker, place vacuum drying oven to carry out drying then, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 18Pa, time of drying, 60min got after the drying: white crystal, that is: anti--2-(2-acetoxy-styrene base)-8-acetoxyl group quinoline;
(3) anti-synthetic-2-(2-hydroxystyrene based)-oxine zinc
1. synthesize in there-necked flask and carry out, there-necked flask is placed on the oil bath cylinder, the oil bath cylinder is placed on the electric heating agitator, nitrogen tube, addition funnel, water cycle prolong are set on there-necked flask from left to right;
2. prepare zinc acetate+aqueous ethanolic solution
1.09g ± 0.001g places beaker with Zinc diacetate dihydrate, adds ethanol 40ml, deionized water 2ml, stirs 5min, becomes: zinc acetate+aqueous ethanolic solution;
3. anti--2-(2-acetoxy-styrene base)-8-acetoxyl group quinoline 3.47g ± 0.001g crystal is placed there-necked flask, add ethanol 30ml, turn on agitator stirs 5min, adds the zinc acetate+aqueous ethanolic solution 42ml ± 1ml of configuration;
Add triethylamine 3ml ± 0.1ml, open the electric heating agitator, temperature rises to 70 ℃ ± 2 ℃ by 25 ℃; To the defeated nitrogen of there-necked flask, nitrogen input speed 20cm
3/ min opens the water cycle prolong, stirs time 120min ± 5min;
In reaction process, chemical reaction will take place, reaction formula is as follows:
In the formula: O: oxygen Zn: zinc
C: carbon H
3C: methyl
N: nitrogen OH: hydroxyl
The reaction back becomes: mixing solutions;
4.. close the electric heating agitator, stop stirring, water cycle condensation, stop to import nitrogen,
Make mixing solutions with 25 ℃ of there-necked flask naturally cooling;
5.. vacuum-drying
Mixing solutions is placed beaker, place vacuum drying oven to carry out drying then, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 18Pa, time of drying, 30min ± 2min got product powder, that is: yellow powder after the drying;
6.. washing with alcohol
Yellow powder is placed beaker, stir 5min, make its precipitation, retain yellow solid product, outwell the ethanol waste liquid with stirring rod;
Washing with alcohol repeats 5 times;
After the washing: yellow solid product;
7.. vacuum-drying
Yellow solid product after the washing with alcohol is placed quartz boat, place vacuum drying oven to carry out drying then, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 10Pa, time of drying, 20min ± 1min got after the drying: yellow powder;
8.. vacuum thermal evaporation is purified
Yellow powder is placed quartz boat, place the vacuum-evaporation stove then, 340 ℃ ± 2 ℃ of Heating temperatures, vacuum tightness 8.5Pa, heat-up time, 240min ± 5min got end product: yellow powder after evaporation is purified;
That is: instead-2-(2-hydroxystyrene based)-oxine zinc yellow toner end;
(4) detect, chemically examine, analyze, characterize
Pattern, color and luster, chemical ingredients, luminescent properties to anti--2-(2-hydroxystyrene based)-oxine zinc product of preparation detect, chemically examine, analyze, characterize;
Carry out Infrared spectroscopy with infrared absorption spectrometer;
Carry out ultraviolet absorption spectroscopy with ultraviolet-visible spectrometer; Carry out the photoluminescence spectra analysis with fluorescence spectrophotometer;
Conclusion: anti--2-(2-hydroxystyrene based)-oxine zinc product is a yellow powder, jaundice green glow, chromaticity coordinates: X=0.4312, Y=0.4861
(5) product stores
Yellow powder product to preparation is stored in the brown transparent Glass Containers, and airtight lucifuge stores, and places cool place, clean environment, waterproof, protection against the tide, sun-proof, acid-proof alkali salt erosion, 20 ℃ ± 2 ℃ of storing temps, relative humidity≤10%.
Beneficial effect
The present invention compares with background technology has tangible advance, be at instead-the synthetic difficult practical situation of 2-(2-hydroxystyrene based)-oxine zinc, adopt two step synthesis methods, synthesize anti--2-(2-acetoxy-styrene base)-8-acetoxyl group quinoline earlier, utilize directly anti-synthetic-2-(2-hydroxystyrene based)-oxine zinc of transesterification reaction then, product is a yellow powder, the jaundice green glow, chromaticity coordinates is X=0.4312, Y=0.4861, the product purity height reaches 99.1%, luminescent properties is good, the production yield rate height reaches 91.7%, this synthetic method craft advanced person, two steps are synthetic rapid and simple, each chemical substance reasonable ratio, processing parameter is accurate, accurately, be the method for directly synthesizing the jaundice green light material with organic+inorganic+vehicle substance.
Description of drawings
Fig. 1 is end product synthetic state figure
Fig. 2 is end product chromaticity coordinates figure
Fig. 3 is end product photoluminescence spectra figure
Fig. 4 is the end product infrared absorpting light spectra
Fig. 5 is the end product uv absorption spectra
Fig. 6 is an end product thermal stability analysis chart
Shown in the figure, list of numerals is as follows:
1. electric heating agitator, 2. display screen, 3. pilot lamp, 4. trip switch, 5. oil bath cylinder, 6. there-necked flask, 7. nitrogen tube, 8. addition funnel, 9. water cycle prolong, 10. air outlet, 11. rising pipes, 12. water inlet pipes, 13. mixing solutions, 14. nitrogengas cylinders, 15. valves, 16. oil bath oil, 17. nitrogen.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing:
Shown in Figure 1, for end product prepares state graph, it is correct that want each position, according to quantity proportioning, operation according to the order of sequence.
The value for preparing required chemical substance is to determine by the scope that sets in advance, and is measure unit with gram, milliliter.
It is clean that the there-necked flask that preparation is used, beaker, stirring rod, container, addition funnel, water cycle prolong etc. will keep, in order to avoid generate by product.
On the top of agitator 1 is oil bath cylinder 5, in oil bath cylinder 5, be oil bath oil 16, on oil bath cylinder 5 tops is there-necked flask 6, on there-necked flask 6, insert nitrogen tube 7, addition funnel 8, water cycle prolong 9 and air outlet 10, rising pipe 11, water inlet pipe 12 from left to right successively, in the there-necked flask 6 is mixing solutions 13, is provided with display screen 2 on electric heating agitator 1, pilot lamp 3, trip switch 4, nitrogen tube 7 connect nitrogengas cylinder 14 and are controlled by valve 15.
Shown in Figure 2, be end product chromaticity coordinates figure, among the figure as can be known: X=0.4312, Y=0.4861, the jaundice green glow.
Shown in Figure 3, be end product fluorescence spectrum distribution plan, among the figure as can be known: ordinate zou is the relative intensity index, and X-coordinate is a wavelength, and unit is nm, and the glow peak main peak is positioned at the 551nm place, and chromaticity coordinates is X=0.4312, Y=0.4861, is a kind of yellow green light emissive material.
Shown in Figure 4, be the end product infrared absorpting light spectra, among the figure as can be known: ordinate zou is a transmitance, and X-coordinate is a wave number, and unit is cm
-1, 3438 (O-H), 3056 (Ar-H), 1630 (C=C), 1557 (C=N), 1507,1439 (Ar-H), 1375,1333 (O-H), 1294,1276,1261 (C-O), 1206,1178,1103 (Ar-H), 960 (trans CH=CH).
Shown in Figure 5, be the uv absorption spectra of end product in ethanol, among the figure as can be known: ordinate zou is the relative intensity index, X-coordinate is a wavelength, unit is nm, absorption peak lays respectively at 304nm, 339nm and 429nm, and the peak at 304nm place obviously is better than other peaks, and 304nm and 339nm belong to the π-π of aromatic nucleus
*Transition, 429nm belongs to n-π
*Transition.
Shown in Figure 6, be end product thermal stability distribution plan, among the figure as can be known: anti--2-(2-hydroxystyrene based)-oxine zinc begins to decompose at 320 ℃, and weightless total residual heavy rate is 64.3% in the time of 800 ℃.
Claims (4)
1. the fast synthesis method of anti--2-(2-hydroxystyrene based)-oxine zinc, it is characterized in that: the chemical substance material of use is: 2-methyl-oxine, zinc acetate, salicylic aldehyde, ethanol, diacetyl oxide, ethyl acetate, triethylamine, deionized water, oil bath oil, nitrogen, its combination consumption is as follows: with gram, milliliter is measure unit
2-methyl-oxine: C
10H
9ON 3.58g ± 0.001g
Zinc acetate: (CH
3COO)
2Zn2H
2O 1.09g ± 0.001g
Salicylic aldehyde: C
7H
6O
22.76g ± 0.001g
Ethanol: C
2H
6O 1000ml ± 10ml
Diacetyl oxide: C
4H
6O
3100ml ± 2ml
Ethyl acetate: C
4H
8O
2200ml ± 5ml
Triethylamine: C
6H
15N 50ml ± 1ml
Deionized water: H
2O 3000ml ± 50ml
Nitrogen: N
220000cm
3± 100cm
3
Oil bath oil: 500ml ± 50ml
Fast synthesis method is as follows:
(1) selected chemical substance material
To carry out selectedly to preparing required chemical substance material, and carry out quality purity control:
2-methyl-oxine: solid-state solid 99.9%
Zinc acetate: solid-state solid 99.8%
Salicylic aldehyde: liquid liquid 99.0%
Ethanol: liquid liquid 99.9%
Diacetyl oxide: liquid liquid 99.9%
Ethyl acetate: liquid liquid 99.9%
Triethylamine: liquid liquid 99.9%
Deionized water: liquid liquid 99.9%
Nitrogen: gaseous state gas 99.8%
Oil bath oil: liquid liquid 90%
(2) anti-synthetic-2-(2-acetoxy-styrene base)-8-acetoxyl group quinoline
1. synthesize in there-necked flask and carry out, there-necked flask is placed on the oil bath cylinder, the oil bath cylinder is placed on the electric heating agitator, on there-necked flask, set gradually nitrogen tube, addition funnel, water cycle prolong from left to right;
Add oil bath oil 800ml in the oil bath cylinder, oil bath oil floods 9/10 of there-necked flask volume;
2. take by weighing salicylic aldehyde 2.76g ± 0.001g;
Take by weighing 2-methyl-oxine 3.58g ± 0.001g;
Take by weighing diacetyl oxide 70ml ± 0.1ml;
Add in the there-necked flask by addition funnel then;
3. open the electric heating agitator, temperature rises to 130 ℃ ± 2 ℃ by 25 ℃, 8 ℃/min of heat-up rate, and stir;
Open nitrogen tube, to there-necked flask input nitrogen, nitrogen input speed 22cm
3/ min;
Open the water cycle prolong, carry out the water cycle condensation;
Limit heating, limit stirring, limit water cycle condensation, limit input nitrogen, time 2400min fully dissolves the interior chemical substance of there-necked flask;
Become: 2-methyl-oxine+salicylic aldehyde+diacetyl oxide ternary mixing solutions;
In synthesis of ternary mixing solutions process, chemical reaction will take place, reaction formula is as follows:
In the formula: O: oxygen H: hydrogen
C: carbon H
3C: methyl
N: nitrogen OH: hydroxyl
4. after reaction finishes, close the electric heating agitator, the water cycle prolong is cooled to 25 ℃ with there-necked flask under nitrogen protection;
5. mixture of ice and water extraction
The preparation mixture of ice and water:
100ml places beaker with deionized water, places refrigerator and cooled to freeze then, makes it form ice cube under-10 ℃;
Add deionized water 100ml in beaker, mix stirring with ice cube, become: mixture of ice and water;
The ternary mixing solutions is added in the beaker, and stir 720min, become: the yellow tertiary mixture aqueous solution with agitator;
6. suction filtration
The tertiary mixture aqueous solution is placed B on the filter flask, carry out suction filtration with two layers of fast qualitative filter paper, retain the product filter cake on the filter paper, and collect, filtrate places filter flask to discard;
7. the washing, suction filtration
The product filter cake is placed beaker, add deionized water 100ml, agitator treating 5min;
Place the B on the filter flask then, carry out suction filtration with two layers of fast qualitative filter paper, retain the product filter cake on the filter paper, filtrate is evacuated in the filter flask and discards;
Washing, suction filtration repeat 5 times;
8. vacuum-drying
The product filter cake is placed quartz boat, place vacuum drying oven to carry out drying then, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 18Pa, time of drying, 60min became after the drying: buff powder;
9. recrystallization is purified
Buff powder is placed another there-necked flask, there-necked flask is placed on the oil bath cylinder, the oil bath cylinder is placed on the electric heating agitator, in there-necked flask, add ethyl acetate 30ml then, turn on agitator, 70 ℃ ± 2 ℃ of Heating temperatures, and carry out the water cycle condensation, heated and stirred 30min becomes: mixing solutions;
While hot mixing solutions is placed on the filter funnel, filter with two layers of fast qualitative filter paper, solution places filter flask;
Filtrate is still aging 120min in filter flask, slowly separates out white crystal;
10.. vacuum-drying
Solution is placed beaker, place vacuum drying oven to carry out drying then, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 18Pa, time of drying, 60min got after the drying: white crystal, that is: anti--2-(2-acetoxy-styrene base)-8-acetoxyl group quinoline;
(3) anti-synthetic-2-(2-hydroxystyrene based)-oxine zinc
1. synthesize in there-necked flask and carry out, there-necked flask is placed on the oil bath cylinder, the oil bath cylinder is placed on the electric heating agitator, nitrogen tube, addition funnel, water cycle prolong are set on there-necked flask from left to right;
2. prepare zinc acetate+aqueous ethanolic solution
Three hydration zinc acetate 1.09g ± 0.001g are placed beaker, add ethanol 40ml, deionized water 2ml, stir 5mmin, become: zinc acetate+aqueous ethanolic solution;
8. anti--2-(2-acetoxy-styrene base)-8-acetoxyl group quinoline 3.47g ± 0.001g crystal is placed there-necked flask, add ethanol 30ml, turn on agitator stirs 5min, adds the zinc acetate+aqueous ethanolic solution 42ml ± 1ml of configuration;
Add triethylamine 3ml ± 0.1ml, open the electric heating agitator, temperature rises to 70 ℃ ± 2 ℃ by 25 ℃; To the defeated nitrogen of there-necked flask, nitrogen input speed 20cm
3/ min opens the water cycle prolong, stirs time 120min ± 5min;
In reaction process, chemical reaction will take place, reaction formula is as follows:
In the formula: O: oxygen Zn: zinc
C: carbon H
3C: methyl
N: nitrogen OH: hydroxyl
The reaction back becomes: mixing solutions;
4.. close the electric heating agitator, stop stirring, water cycle condensation, stop to import nitrogen, make mixing solutions with 25 ℃ of there-necked flask naturally cooling;
5.. vacuum-drying
Mixing solutions is placed beaker, place vacuum drying oven to carry out drying then, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 18Pa, time of drying, 30min ± 2min got product powder, that is: yellow powder after the drying;
6.. washing with alcohol
Yellow powder is placed beaker, stir 5min, make its precipitation, retain yellow solid product, outwell the ethanol waste liquid with stirring rod;
Washing with alcohol repeats 5 times;
After the washing: yellow solid product;
7.. vacuum-drying
Yellow solid product after the washing with alcohol is placed quartz boat, place vacuum drying oven to carry out drying then, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 10Pa, time of drying, 20min ± 1min got after the drying: yellow powder;
8.. vacuum thermal evaporation is purified
Yellow powder is placed quartz boat, place the vacuum-evaporation stove then, 340 ℃ ± 2 ℃ of Heating temperatures, vacuum tightness 8.5Pa, heat-up time, 240min ± 5min got end product: yellow powder after evaporation is purified;
That is: instead-2-(2-hydroxystyrene based)-oxine zinc yellow toner end;
(4) detect, chemically examine, analyze, characterize
Pattern, color and luster, chemical ingredients, luminescent properties to anti--2-(2-hydroxystyrene based)-oxine zinc product of preparation detect, chemically examine, analyze, characterize;
Carry out Infrared spectroscopy with infrared absorption spectrometer;
Carry out ultraviolet absorption spectroscopy with ultraviolet-visible spectrometer;
Carry out the photoluminescence spectra analysis with fluorescence spectrophotometer;
Conclusion: anti--2-(2-hydroxystyrene based)-oxine zinc product is a yellow powder, jaundice green glow, chromaticity coordinates: X=0.4312, Y=0.4861
(5) product stores
Yellow powder product to preparation is stored in the brown transparent Glass Containers, and airtight lucifuge stores, and places cool place, clean environment, waterproof, protection against the tide, sun-proof, acid-proof alkali salt erosion, 20 ℃ ± 2 ℃ of storing temps, relative humidity≤10%.
2. according to claim 1 a kind of anti--fast synthesis method of 2-(2-hydroxystyrene based)-oxine zinc, it is characterized in that: described anti--2-(2-hydroxystyrene based)-oxine zinc preparation carries out in there-necked flask, be to stir at electric heating, the water cycle condensation, finish under the oil bath, on the top of agitator (1) is oil bath cylinder (5), in oil bath cylinder (5), be oil bath oil (16), on oil bath cylinder (5) top is there-necked flask (6), on there-necked flask (6), insert nitrogen tube (7) from left to right successively, addition funnel (8), water cycle prolong (9) and air outlet (10), rising pipe (11), water inlet pipe (12), in the there-necked flask (6) is mixing solutions (13), on electric heating agitator (1), be provided with display screen (2), pilot lamp (3), trip switch (4), nitrogen tube (7) connect nitrogengas cylinder (14) and are controlled by valve (15).
3. according to claim 1 a kind of anti--fast synthesis method of 2-(2-hydroxystyrene based)-oxine zinc, it is characterized in that: described anti--2-(2-hydroxystyrene based)-oxine zinc photoluminescence spectra maximum emission wavelength is 551nm, halfwidth is 78nm.
4. according to claim 1 a kind of anti--fast synthesis method of 2-(2-hydroxystyrene based)-oxine zinc, it is characterized in that: anti--2-(2-hydroxystyrene based)-oxine zinc begins to decompose at 320 ℃, and weightless total residual heavy rate is 64.3% in the time of 800 ℃.
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Cited By (3)
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| CN103642489A (en) * | 2013-12-24 | 2014-03-19 | 贵州大学 | Quinaldine derivative a fluorescent reagent as well as preparation method and application thereof |
| CN103641779A (en) * | 2013-12-24 | 2014-03-19 | 贵州大学 | Quinaldine derivative b fluorescent and colorimetric reagent as well as preparation method and application thereof |
| CN105019013A (en) * | 2015-06-30 | 2015-11-04 | 太原理工大学 | Blue-light emitting monocrystalline material preparation method |
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| 卫芳芳等: "《8-羟基喹啉金属配合物的制备与提纯》", 《人工晶体学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103642489A (en) * | 2013-12-24 | 2014-03-19 | 贵州大学 | Quinaldine derivative a fluorescent reagent as well as preparation method and application thereof |
| CN103641779A (en) * | 2013-12-24 | 2014-03-19 | 贵州大学 | Quinaldine derivative b fluorescent and colorimetric reagent as well as preparation method and application thereof |
| CN103642489B (en) * | 2013-12-24 | 2015-01-21 | 贵州大学 | Quinaldine derivative a fluorescent reagent as well as preparation method and application thereof |
| CN105019013A (en) * | 2015-06-30 | 2015-11-04 | 太原理工大学 | Blue-light emitting monocrystalline material preparation method |
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|---|---|
| CN102153570B (en) | 2013-06-12 |
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