CN1059657C - Method for refining beta-methyl naphthalene from coal-tar oil crude methyl naphthalene - Google Patents
Method for refining beta-methyl naphthalene from coal-tar oil crude methyl naphthalene Download PDFInfo
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- CN1059657C CN1059657C CN96117039A CN96117039A CN1059657C CN 1059657 C CN1059657 C CN 1059657C CN 96117039 A CN96117039 A CN 96117039A CN 96117039 A CN96117039 A CN 96117039A CN 1059657 C CN1059657 C CN 1059657C
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- methylnaphthalene
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- glycol ether
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Abstract
The present invention discloses a method for refining crude methylnaphthalene recovered from coal tar into beta-methylnaphthalene. After simple acid washing and quinoline removing, the crude methylnaphthalene recovered from coal tar is enriched and distilled; then, diethylene glycol is added into the crude methylnaphthalene for azeotropic distillation; finally, refined beta-methylnaphthalene with the content higher than 95% is obtained through rectification. The crystallizing point of the beta-methylnaphthalene obtained by the method of the present invention is higher than 30 DEG C, and the beta-methylnaphthalene obtained by the method has micro quinoline and indole impurity content. The method of the present invention meets the requirement of fine chemistry industry.
Description
The present invention relates to the processing of coal tar, particularly relate to azeotropic distn refining beta-methylnaphthalene from the coal tar crude methylnaphthalene.
The thick methylnaphthalene that reclaims from coal tar contains beta-methylnaphthalene about 50%, and alpha-methyl-naphthalene about 20% also has a spot of naphthalene, quinoline, indoles, biphenyl etc. in addition.Because beta-methylnaphthalene and alpha-methyl-naphthalene boiling point are approaching, and quinoline, indoles and beta-methylnaphthalene have azeotropism, therefore be difficult to the high beta-methylnaphthalene of production purity with common distillating method, present domestic employing is earlier with thick methylnaphthalene enrichment distillation, the content of beta-methylnaphthalene is brought up to more than 70%, separate alpha-methyl-naphthalene and beta-methylnaphthalene with perfectly crystallization process then, the ctystallizing point of the beta-methylnaphthalene of producing can reach 28 ℃, but the indoles that contains 1-2% in the product, vitamin K with this beta-methylnaphthalene production has stink, need remove alkaline matters such as indoles with hydrochloric acid, production technique falls behind in advance, and labor condition is poor, product purity is not high.
The Japanese Patent spy opens the process for purification that clear 62-153232 discloses a kind of beta-methylnaphthalene, adds thanomin or alcamines in the organic mixture that contains beta-methylnaphthalene and alpha-methyl-naphthalene, carries out the process for purification of the beta-methylnaphthalene of component distillation again.The content of beta-methylnaphthalene in the unqualified raw material of this method, but actual when adopting this method, effect was all bad when the content of beta-methylnaphthalene was too low or too high in the raw material, and this method do not consider the recovery of entrainer, and production cost is improved.In addition, among the embodiment of this method, strict to processing condition control, the cut that cuts during distillation reaches 9 more than, and needs to adopt centrifugal separation to obtain beta-methylnaphthalene behind the crystallisation by cooling.So this method complicated operation, processing step is many, and the raw material composition is difficult for holding, and entrainer consumption is big, and these all are unfavorable for suitability for industrialized production.
The objective of the invention is to be to provide a kind of technological operation step simple, because the recovery of entrainer is reused, production cost is minimized, the purity height of product is suitable for the process for purification of the beta-methylnaphthalene of suitability for industrialized production.
Concrete technical scheme of the present invention be earlier with coal tar through distillation, simple acid strips the thick methylnaphthalene (wherein the content of beta-methylnaphthalene is about 50% weight ratio) that quinoline obtains and carries out the enrichment distillation, cut the beta-methylnaphthalene enriched fraction at tower top temperature 240-242 ℃, add weight then and carry out component distillation as entrainer for the glycol ether of this enriched fraction 30-50%, cut beta-methylnaphthalene middle runnings at tower top temperature 224-230 ℃, the middle runnings of beta-methylnaphthalene is left standstill, glycol ether and beta-methylnaphthalene layering, divide and remove glycol ether, at last with this middle runnings rectifying, cut out ctystallizing point more than or equal to 30 ℃ beta-methylnaphthalene at tower top temperature 240-242 ℃.
Overhead product is heterogeneous state during component distillation, is divided into two layers, and the upper strata material is middle runnings, the bigger glycol ether of proportion is in lower floor, can reclaim and do entrainer continuation use, after the middle runnings of beta-methylnaphthalene cuts, return recyclable remaining entrainer in the still with mixed methylnaphthalene.The content of remaining entrainer can be below 2% weight ratio in the still.
The present invention has avoided the distillation crystallization need use the shortcoming of a large amount of acid solutions, compare with Japanese documentation, it is simple to have operating procedure, entrainer is recyclable, make production cost reduce, and the purity height of the beta-methylnaphthalene of the present invention's acquisition, ctystallizing point can reach more than 30 ℃, is suitable for suitability for industrialized production and uses.
Embodiment: use 25, H1500mm strap clamp cover glass distillation tower, stainless steel triangle filler, the high 1300mm of filler, three mouthfuls of distilling flasks, the heating of 2KW electric furnace, transformer regulation and control.
With coal tar through distillation, the thick methylnaphthalene that obtains after stripping quinoline of acid, carry out the enrichment distillation, at tower top temperature 240-241 ℃ of enriched fraction that cuts beta-methylnaphthalene.Get beta-methylnaphthalene enriched fraction 800 gram, glycol ether 400 grams drop in the stills, and reflux ratio is at 7-20: adjusting 1 scope in, carry out component distillation, and its recovered temperature and overhead product component content see Table 1.Table 1
| The fraction title | Form % | Productive rate % | ||||||
| Naphthalene | Quinoline | Glycol ether | Indoles | Beta-methylnaphthalene | Alpha-methyl-naphthalene | Unknown | ||
| Enrichment fraction raw material | 0.24 | 1.87 | 3.95 | 84.97 | 6.29 | 2.68 | ||
| Foreshot 200-225 ℃ | 3.8 | 2.3 | 1.7 | 80.54 | 2.1 | 9.86 | 9.38 | |
| 225-230 ℃ of beta-methylnaphthalene middle distillate | 0.6 | 0.15 | 1.6 | 0.1 | 91.62 | 4.7 | 1.23 | 50.4 |
| Reclaim entrainer | Do not analyze | 21.89 | ||||||
| Still is residual | Do not analyze | 18.33 | ||||||
After the middle runnings of 225 ℃ of beta-methylnaphthalenes cuts, return recyclable remaining entrainer in the still with mixed methylnaphthalene.The content that makes remaining entrainer in the still is below 2% weight ratio.The overhead product of this component distillation is heterogeneous state, is divided into two layers, and the upper strata material is middle runnings, and lower floor is the bigger glycol ether of proportion, with the separatory means it is separated, and glycol ether can be made entrainer and use.
2. get beta-methylnaphthalene middle runnings 1000 gram and drop in the stills and carry out rectifying, reflux ratio is at 5-10: adjusting 1 scope in, the temperature of its overhead product and overhead product component content see Table 2.Table 2
| The fraction title | Form % | Productive rate % | ||||||
| Naphthalene | Quinoline | Glycol ether | Indoles | Beta-methylnaphthalene | Alpha-methyl-naphthalene | Unknown | ||
| Raw material Beta-methyl middle distillate | 0.6 | 0.15 | 1.6 | 0.1 | 91.62 | 4.7 | 1.23 | |
| Foreshot 200-235 ℃ | 1.2 | 2.2 | 80.3 | 2.4 | 13.9 | 13.4 | ||
| Middle distillate 235-240 ℃ | 0.1 | 1.5 | 92.4 | 1.5 | 4.5 | 25.5 | ||
| 240-242 ℃ of beta-methylnaphthalene product | 0.01 | 95.8 | 3.1 | 1.09 | 51.3 | |||
| Still is residual | 9.8 | |||||||
Claims (3)
1, a kind of method from coal tar crude refining beta-methyl naphthalene-methylnaphthalene, it is characterized in that may further comprise the steps successively: (1) obtains through distillation, acid coal tar after stripping quinoline thick methylnaphthalene carries out the enrichment distillation, cuts the beta-methylnaphthalene enriched fraction for 240～242 ℃ in tower top temperature; (2) in this enriched fraction, add weight and carry out component distillation, in 224～230 ℃ of middle runningss that cut beta-methylnaphthalene of tower top temperature for the glycol ether of this enriched fraction 30%～50%; (3) middle runnings of beta-methylnaphthalene is left standstill, glycol ether and beta-methylnaphthalene layering divide and to remove glycol ether, go the beta-methylnaphthalene middle runnings of glycol ether refining branch, cut out ctystallizing point more than or equal to 30 ℃ beta-methylnaphthalene 240～242 ℃ of tower top temperatures.
2, the method for refining beta-methylnaphthalene according to claim 1, it is characterized in that the overhead product layering of component distillation in the step (2) after, the glycol ether of lower floor can reclaim as entrainer and continue to use.
3, the method for refining beta-methylnaphthalene according to claim 1, it is characterized in that beta-methylnaphthalene middle runnings cuts in the step (2) after, mixed methylnaphthalene returned reclaims remaining entrainer in the still.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96117039A CN1059657C (en) | 1996-07-26 | 1996-07-26 | Method for refining beta-methyl naphthalene from coal-tar oil crude methyl naphthalene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96117039A CN1059657C (en) | 1996-07-26 | 1996-07-26 | Method for refining beta-methyl naphthalene from coal-tar oil crude methyl naphthalene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1172096A CN1172096A (en) | 1998-02-04 |
| CN1059657C true CN1059657C (en) | 2000-12-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96117039A Expired - Lifetime CN1059657C (en) | 1996-07-26 | 1996-07-26 | Method for refining beta-methyl naphthalene from coal-tar oil crude methyl naphthalene |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100535079C (en) * | 2005-06-22 | 2009-09-02 | 上海宝钢化工有限公司 | Method for removing indole from coal tar downstream fraction or product |
| CN106146245A (en) * | 2015-03-28 | 2016-11-23 | 鞍钢股份有限公司 | A kind of method using continuous azeotropic distillation technique to produce beta-methylnaphthalene |
| CN114394880A (en) * | 2022-02-14 | 2022-04-26 | 煤炭科学技术研究院有限公司 | Method for extracting high-purity 2-methylnaphthalene from wash oil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6036427A (en) * | 1983-08-08 | 1985-02-25 | Sumikin Coke Co Ltd | Separation of methylnaphthalene from hydrocarbon oil containing methylnaphthalene |
| EP0518294A1 (en) * | 1991-06-11 | 1992-12-16 | Kawasaki Steel Corporation | Method for refining methylnaphthalene containing oil |
-
1996
- 1996-07-26 CN CN96117039A patent/CN1059657C/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6036427A (en) * | 1983-08-08 | 1985-02-25 | Sumikin Coke Co Ltd | Separation of methylnaphthalene from hydrocarbon oil containing methylnaphthalene |
| EP0518294A1 (en) * | 1991-06-11 | 1992-12-16 | Kawasaki Steel Corporation | Method for refining methylnaphthalene containing oil |
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| Publication number | Publication date |
|---|---|
| CN1172096A (en) | 1998-02-04 |
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