CN101665402B - Preparation method of refined fluorene - Google Patents
Preparation method of refined fluorene Download PDFInfo
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- CN101665402B CN101665402B CN 200810013045 CN200810013045A CN101665402B CN 101665402 B CN101665402 B CN 101665402B CN 200810013045 CN200810013045 CN 200810013045 CN 200810013045 A CN200810013045 A CN 200810013045A CN 101665402 B CN101665402 B CN 101665402B
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- necked flask
- crystallization
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- chlorobenzene
- filtrate
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- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- NIHNNTQXNPWCJQ-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 title abstract 20
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Substances ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims abstract description 72
- 238000002425 crystallisation Methods 0.000 claims abstract description 58
- 230000008025 crystallization Effects 0.000 claims abstract description 56
- 239000000706 filtrate Substances 0.000 claims abstract description 43
- 239000000047 product Substances 0.000 claims abstract description 37
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 37
- 239000002904 solvent Substances 0.000 claims abstract description 33
- 238000001816 cooling Methods 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 21
- MVPPADPHJFYWMZ-IDEBNGHGSA-N chlorobenzene Chemical group Cl[13C]1=[13CH][13CH]=[13CH][13CH]=[13CH]1 MVPPADPHJFYWMZ-IDEBNGHGSA-N 0.000 claims abstract description 8
- 238000004821 distillation Methods 0.000 claims abstract description 7
- 238000011084 recovery Methods 0.000 claims abstract description 7
- 150000002220 fluorenes Chemical class 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 32
- 238000001914 filtration Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000003760 magnetic stirring Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 8
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 25
- TXCDCPKCNAJMEE-UHFFFAOYSA-N dibenzofuran Chemical group C1=CC=C2C3=CC=CC=C3OC2=C1 TXCDCPKCNAJMEE-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- GGXKQILBNJUKSH-UHFFFAOYSA-N 1-methyldibenzofuran Chemical compound O1C2=CC=CC=C2C2=C1C=CC=C2C GGXKQILBNJUKSH-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000011280 coal tar Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a preparation method of refined fluorene, which comprises the steps of taking industrial fluorene as a raw material, taking secondary, tertiary and quaternary chlorobenzene filtrate and chlorobenzene as solvents, carrying out programmed cooling crystallization at a speed of 0.5-4 ℃/min after dissolving at a temperature of 40-90 ℃ for 40-90 min, wherein the final crystallization temperature is 15-40 ℃, then carrying out vacuum filtration, and carrying out crystallization for four times to obtain a refined fluorene product with the content of more than 99%. The purity of the refined fluorene product can reach more than 99%, and the extraction rate of the refined fluorene can reach more than 75%. Meanwhile, the chlorobenzene filtrate is recycled without distillation, and a large amount of fluorene fraction can be recovered. Except the primary filtrate, other filtrates can be recycled, so that the recovery amount of the solvent is reduced. According to the calculation of processing 100 tons of industrial fluorene every year, 75 tons of refined fluorene can be produced every year, and the economic benefit reaches 300 ten thousand yuan. And the raw material industrial fluorene has rich resources, low price, relatively simple preparation process and convenient mastering and operation.
Description
Technical field
The invention belongs to coal chemical technology, relate in particular to a kind of tar byproduct industry fluorenes that utilizes and produce the method that content reaches smart fluorenes more than 99%.
Background technology
The industry fluorenes is one of byproduct of coke-oven plant's coal tar, accounts for 1%～2% of coal tar, and the output of China's industry fluorenes is very large, and therefore the price of industrial fluorenes is also very cheap.In recent years, more and more extensive in the application in the fields such as chemical industry, biotechnology, polymer synthetic chemistry and functional high molecule material by the derivative that fluorenes is synthetic, the domestic and international market is to the demand rapid growth of fluorenes, particularly grow with each passing day especially to the demand of smart fluorenes in the foreign market, and prospect is very wide.
The boiling point of fluorenes is 297 ℃, and fusing point is 115 ℃, and its major impurity is dibenzofuran and methyl dibenzofuran.Because the boiling-point difference of dibenzofuran and methyl dibenzofuran and fluorenes is very little, only have about 8 ℃, so the refining of fluorenes substantially all is to take chemically separated method.At present, the industrial fluorenes separating and purifying method of producing smart fluorenes roughly has following three kinds:
1, solvent crystallization: the method for namely using the dissolution with solvents post crystallization.Because used solvent is different, quality product is also different from yield, and the solvent of employing has respectively benzene, toluene, chlorobenzene, painter's naphtha and dimethyl formamide etc., and this method is used general, easy handling; But solvent consumption is larger, makes to produce the cost increase.
2, crystallisation by cooling method: behind the first crystallisation by cooling, use the method for solvent wash, the fluorenes product content that this method is produced is lower, does not reach purity requirement again.
3, perfectly crystallization process: obtain fluorenes by the material decrease temperature crystalline.Though this method is simple, the fluorenes purity of producing is only used about 80%.
Aforesaid method cuts both ways, and is therefore also just more urgent and need to the research of smart fluorenes preparation method.
Summary of the invention
Purpose of the present invention is maximized favourable factors and minimized unfavourable ones exactly, recycles chlorobenzene filtrate and chlorobenzene is made solvent, through dissolving, cooling, suction filtration and four crystallizations, makes content greater than 99% smart fluorenes product.
The technical solution that the present invention takes is:
A kind of preparation method of smart fluorenes, take industrial fluorenes as raw material, make solvent with secondary chlorobenzene filtrate, three chlorobenzene filtrate, four chlorobenzene filtrate and chlorobenzene, 40～90 ℃ of solvent temperatures, behind dissolution time 40～90min, carry out the programmed cooling crystallization with the speed of 0.5 ℃/min～4 ℃/min, the crystallization final temperature is controlled between 15～40 ℃, then carry out vacuum filtration, through four crystallizations, obtain content greater than 99% smart fluorenes product.
Its reparation technology process is:
For the first time crystallization: primary industry fluorenes and the secondary chlorobenzene filtrate ratio according to 1:0.5～3 is respectively charged in the there-necked flask; There-necked flask is immersed in the water-bath, installs magnetic stirring apparatus, beginning heat temperature raising, and uninterrupted the stirring; Between 50～90 ℃ of temperature, when raw material and solvent all after the dissolving, keep constant temperature 50～90min; Then mixing solutions start program cooling, cooling rate are 0.5 ℃/min～4 ℃/min, and crystallization slowly occurs; Temperature drops to after 15～40 ℃, and there-necked flask is taken out from water-bath: the mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Be the primary crystallization product behind the filtration cakes torrefaction; Filtrate is reused through behind the Distillation recovery;
For the second time crystallization: primary crystallization product and three chlorobenzene filtrate or chlorobenzene are packed in the there-necked flask according to the ratio of 1:0.5～3; There-necked flask is immersed in the water-bath, installs magnetic stirring apparatus, beginning heat temperature raising, and uninterrupted the stirring; Between 45～85 ℃ of temperature, when raw material and solvent all after the dissolving, keep constant temperature 40～90min; Then mixing solutions start program cooling, cooling rate are 0.5 ℃/min～4 ℃/min, and crystallization slowly occurs; Temperature is taken out there-necked flask after dropping to 15～40 ℃ from water-bath; Mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Be the secondary crystal product behind the filtration cakes torrefaction; The filtrate direct circulation uses;
For the third time crystallization: secondary crystal product and four chlorobenzene filtrate or chlorobenzene are packed in the there-necked flask according to the ratio of 1:0.5～3; There-necked flask is immersed in the water-bath, installs magnetic stirring apparatus, beginning heat temperature raising, and uninterrupted the stirring; Between 40～80 ℃ of temperature, when raw material and solvent all after the dissolving, keep constant temperature 40～90min; Then mixing solutions start program cooling, cooling rate are 0.5 ℃/min～4 ℃/min, and crystallization slowly occurs; Temperature is taken out there-necked flask after dropping to 15～40 ℃ from water-bath; Mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Be crystallized product behind the filtration cakes torrefaction three times; The filtrate direct circulation uses;
The 4th crystallization: three crystallized products and chlorobenzene are packed in the there-necked flask according to the ratio of 1:0.5～3; There-necked flask is immersed in the water-bath, installs magnetic stirring apparatus, beginning heat temperature raising, and uninterrupted the stirring; Between 40～80 ℃ of temperature, when raw material and solvent all after the dissolving, keep constant temperature 50～90min; Then mixing solutions start program cooling, cooling rate are 0.5 ℃/min～4 ℃/min, and crystallization slowly occurs; Temperature is taken out there-necked flask after dropping to 15～40 ℃ from water-bath; Mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Be content behind the filtration cakes torrefaction greater than 99% smart fluorenes product; Filtrate is continued direct circulation and is used.
Beneficial effect of the present invention is:
Implement the present invention, the one, the smart fluorenes product purity of gained is high, can guarantee that content reaches more than 99%.The 2nd, the product recovery rate is high, and more than the smart fluorenes extraction rate reached to 75, chlorobenzene filtrate can be recycled without Distillation recovery simultaneously, can reclaim wherein a large amount of fluorenes cuts.The 3rd, the quantity of solvent recuperation is few, and except first-time filtrate, the equal reusable edible of other filtrates has greatly reduced the yield of solvent.The 4th, comprehensive benefit is considerable, according to processing 100 tons of industrial fluorenes, extraction yield 75% calculating year, can produce 75 tons of smart fluorenes per year, and economic benefit reaches 3,000,000 yuan.The 5th, primary industry fluorenes aboundresources, cheap, and reparation technology is relatively simple, is convenient to grasp and operation.
Embodiment
Below, in conjunction with the embodiments the present invention is further described.
The preparation method of the present invention's smart fluorenes, as raw material take industrial fluorenes, take secondary chlorobenzene filtrate, three chlorobenzene filtrate, four chlorobenzene filtrate and an amount of chlorobenzene as solvent, solvent temperature is controlled between 40～90 ℃, behind constant temperature dissolving 40～90min, carries out the programmed cooling crystallization with the speed of 0.5 ℃/min～4 ℃/min, the crystallization control final temperature is between 15～40 ℃, carry out vacuum filtration with the vacuum filtration device, through four crystallizations, obtain content greater than 99% smart fluorenes product.
Embodiment 1:
For the first time crystallization: primary industry fluorenes and secondary chlorobenzene filtrate are packed in the there-necked flask according to the ratio of 1:3.Then there-necked flask is immersed in the water-bath; Install magnetic stirring apparatus, while stirring heat temperature raising.Treat that temperature reaches 50 ℃, after raw material and solvent all dissolved, constant temperature kept 90min.Then, with the cooling rate of 4 ℃/min the mixing solutions start program is lowered the temperature, crystallization slowly appears in mixed solution.After continuing to be cooled to 40 ℃, there-necked flask is taken out from water-bath.At last, the mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Be the primary crystallization product behind the filtration cakes torrefaction.Filtrate is reused through behind the Distillation recovery.
For the second time crystallization: primary crystallization product and three chlorobenzene filtrate are packed in the there-necked flask according to the ratio of 1:2; There-necked flask is immersed in the water-bath, installs magnetic stirring apparatus, while stirring heat temperature raising.Treat that temperature reaches 85 ℃, raw material and solvent keep constant temperature 75min after all dissolving; Then, with the cooling rate of 0.5 ℃/min the mixing solutions start program is lowered the temperature, crystallization slowly occurs; Temperature is taken out there-necked flask after being down to 25 ℃ from water-bath; Mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Be the secondary crystal product behind the filtration cakes torrefaction.Filtrate not Distillation recovery and direct circulation is used.
For the third time crystallization: secondary crystal product and four chlorobenzene filtrate or chlorobenzene are packed in the there-necked flask according to the ratio of 1:2.5; There-necked flask is immersed in the water-bath, installs magnetic stirring apparatus, while stirring heat temperature raising.Treat that temperature reaches 40 ℃, raw material and solvent keep constant temperature 40min after all dissolving; With the cooling rate team mixing solutions start program cooling of 0.5 ℃/min, slowly crystallization; Temperature is taken out there-necked flask after dropping to 20 ℃ from water-bath; Mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration, be crystallized product behind the filtration cakes torrefaction three times.Filtrate is not reclaimed and is continued the direct circulation use,
The 4th crystallization: three crystallized products and chlorobenzene are packed in the there-necked flask according to the ratio of 1:0.5; There-necked flask is immersed in the water-bath, installs magnetic stirring apparatus, heat temperature raising reaches 40 ℃ in temperature while stirring, and raw material and solvent keep constant temperature 60min after all dissolving; Then with the cooling rate start program cooling of mixing solutions with 2 ℃/min, crystallization slowly occurs; Temperature is taken out there-necked flask after dropping to 30 ℃ from water-bath; Mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Namely make content behind the filtration cakes torrefaction greater than 99% smart fluorenes product.Filtrate then can be continued direct circulation and be used.
Embodiment 2:
For the first time crystallization: primary industry fluorenes and secondary chlorobenzene filtrate are packed in the there-necked flask according to the ratio of 1:0.5; There-necked flask is immersed in the water-bath, while stirring heat temperature raising; Temperature rises to 90 ℃, and raw material and solvent keep constant temperature 50min after all dissolving; Then mixing solutions start program cooling, cooling rate is 0.5 ℃/min, crystallization slowly occurs; Temperature drops to after 15 ℃, and there-necked flask is taken out from water-bath: the mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Be the primary crystallization product behind the filtration cakes torrefaction.Filtrate is reused through behind the Distillation recovery.
For the second time crystallization: primary crystallization product and chlorobenzene are packed in the there-necked flask according to the ratio of 1:0.5; There-necked flask is immersed in the water-bath, installs magnetic stirring apparatus, be heated to while stirring 45 ℃, raw material and solvent keep constant temperature 40min after all dissolving; Then mixing solutions start program cooling, cooling rate is 4 ℃/min, crystallization slowly occurs; Temperature is taken out there-necked flask after dropping to 15 ℃ from water-bath; Mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Be the secondary crystal product behind the filtration cakes torrefaction.Filtrate is not reclaimed direct circulation and is used.
For the third time crystallization: secondary crystal product and four chlorobenzene filtrate are packed in the there-necked flask according to the ratio of 1:1.5; There-necked flask is immersed in the water-bath, is heated to while stirring 45 ℃, raw material and solvent keep constant temperature 70min after all dissolving; Then mixing solutions start program cooling, cooling rate is 4 ℃/min, crystallization slowly occurs; Temperature is taken out there-necked flask after dropping to 40 ℃ from water-bath; Mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Be crystallized product behind the filtration cakes torrefaction three times.Filtrate is not reclaimed direct circulation and is used.
The 4th crystallization: three crystallized products and chlorobenzene are packed in the there-necked flask according to the ratio of 1:3; There-necked flask is immersed in the water-bath, installs magnetic stirring apparatus, be heated to while stirring 45 ℃, raw material and solvent keep constant temperature 90min after all dissolving; Then mixing solutions begins cooling by the cooling rate of 0.5 ℃/min, and crystallization slowly occurs; Temperature is taken out there-necked flask after dropping to 15 ℃ from water-bath; Mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Namely make content behind the filtration cakes torrefaction greater than 99% smart fluorenes product.
Claims (1)
1. the preparation method of a smart fluorenes, take industrial fluorenes as raw material, make solvent with secondary chlorobenzene filtrate, three chlorobenzene filtrate, four chlorobenzene filtrate and chlorobenzene, 40～90 ℃ of solvent temperatures, behind dissolution time 40～90min, carry out the programmed cooling crystallization with the speed of 0.5 ℃/min～4 ℃/min, the crystallization final temperature is controlled between 15～40 ℃, then carry out vacuum filtration, through four crystallizations, obtain content greater than 99% smart fluorenes product; It produces process:
For the first time crystallization: primary industry fluorenes and secondary chlorobenzene filtrate are respectively charged in the there-necked flask according to 1: 0.5～3 ratio; There-necked flask is immersed in the water-bath, installs magnetic stirring apparatus, beginning heat temperature raising, and uninterrupted the stirring; Between 50～90 ℃ of temperature, when raw material and solvent all after the dissolving, keep constant temperature 50～90min; Then mixing solutions start program cooling, cooling rate are 0.5 ℃/min～4 ℃/min, and crystallization slowly occurs; Temperature drops to after 15～40 ℃, and there-necked flask is taken out from water-bath: the mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Be the primary crystallization product behind the filtration cakes torrefaction; Filtrate is reused through behind the Distillation recovery;
For the second time crystallization: primary crystallization product and three chlorobenzene filtrate or chlorobenzene are packed in the there-necked flask according to 1: 0.5～3 ratio; There-necked flask is immersed in the water-bath, installs magnetic stirring apparatus, beginning heat temperature raising, and uninterrupted the stirring; Between 45～85 ℃ of temperature, when raw material and solvent all after the dissolving, keep constant temperature 40～90min; Then mixing solutions start program cooling, cooling rate are 0.5 ℃/min～4 ℃/min, and crystallization slowly occurs; Temperature is taken out there-necked flask after dropping to 15～40 ℃ from water-bath; Mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Be the secondary crystal product behind the filtration cakes torrefaction; The filtrate direct circulation uses;
For the third time crystallization: secondary crystal product and four chlorobenzene filtrate or chlorobenzene are packed in the there-necked flask according to 1: 0.5～3 ratio; There-necked flask is immersed in the water-bath, installs magnetic stirring apparatus, beginning heat temperature raising, and uninterrupted the stirring; Between 40～80 ℃ of temperature, when raw material and solvent all after the dissolving, keep constant temperature 40～90min; Then mixing solutions start program cooling, cooling rate are 0.5 ℃/min～4 ℃/min, and crystallization slowly occurs; Temperature is taken out there-necked flask after dropping to 15～40 ℃ from water-bath; Mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Be crystallized product behind the filtration cakes torrefaction three times; The filtrate direct circulation uses;
The 4th crystallization: three crystallized products and chlorobenzene are packed in the there-necked flask according to 1: 0.5～3 ratio; There-necked flask is immersed in the water-bath, installs magnetic stirring apparatus, beginning heat temperature raising, and uninterrupted the stirring; Between 40～80 ℃ of temperature, when raw material and solvent all after the dissolving, keep constant temperature 50～90min; Then mixing solutions start program cooling, cooling rate are 0.5 ℃/min～4 ℃/min, and crystallization slowly occurs; Temperature is taken out there-necked flask after dropping to 15～40 ℃ from water-bath; Mixing solutions in the there-necked flask is poured in the prior mounted vacuum filtration device, carried out vacuum filtration; Be content behind the filtration cakes torrefaction greater than 99% smart fluorenes product; Filtrate is continued direct circulation and is used.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1651367A (en) * | 2004-12-07 | 2005-08-10 | 哈尔滨工程大学 | Method of extracting high purity acenaphthene from coat tar scrubbing oil |
| CN1884234A (en) * | 2005-06-22 | 2006-12-27 | 上海宝钢化工有限公司 | Method for purifying fluorene crystals |
| CN101177372A (en) * | 2007-12-12 | 2008-05-14 | 卫宏远 | Method for purifying pure acenaphthene |
| CN101182278A (en) * | 2007-12-12 | 2008-05-21 | 卫宏远 | Method for purifying refined fluorene by crystallizing process |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1651367A (en) * | 2004-12-07 | 2005-08-10 | 哈尔滨工程大学 | Method of extracting high purity acenaphthene from coat tar scrubbing oil |
| CN1884234A (en) * | 2005-06-22 | 2006-12-27 | 上海宝钢化工有限公司 | Method for purifying fluorene crystals |
| CN101177372A (en) * | 2007-12-12 | 2008-05-14 | 卫宏远 | Method for purifying pure acenaphthene |
| CN101182278A (en) * | 2007-12-12 | 2008-05-21 | 卫宏远 | Method for purifying refined fluorene by crystallizing process |
Non-Patent Citations (1)
| Title |
|---|
| 龚俊库.溶剂结晶法制取精芴的研究.《燃料与化工》.1998,第29卷(第4期),第213-215页. * |
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