Method for recovering m-cresol from mixture containing n-cresols

专利摘要:
In a method for recovery of m-cresol from its mixture with at least one material which is not reacted with urea which comprises treating the said mixture with urea at a lower temperature to form a molecular compound of m-cresol and urea, separating the molecular compound from the resulting mixture, decomposing the molecular compound at a higher temperature to m-cresol and urea and separating m-cresol from the resultant mixture, an improvement that at least one of the steps of formation and the decomposition of the molecular compound is carried out in a solvent selected from the group consisting of benzenes substituted or not with 1 to 3 alkyl groups of 1 to 4 carbon atoms and/or 1 or 2 halogen atoms, dialkyl ethers of which the alkyl moiety has 2 to 5 carbon atoms and cyclic ethers having 4 or 5 carbon atoms, whereby m-cresol is recovered quantitatively in a highly pure state.
公开号:SU1053741A3
申请号:SU711686002
申请日:1971-07-21
公开日:1983-11-07
发明作者:Суда Хидеаки；Дохгане Ивао；Хосака Хироказу；Эбара Козунари
申请人:Сумитомо Кемикал Компани,Лимитед (Фирма)；
IPC主号:

专利说明:

The invention relates to an improved method for separating f -cr ash from a mixture containing m- and ncc ashes. m -Cresol is widely used in the production of synthetic fragrances, in the production of plastics. A method is known for isolating M-chrome ash from a mixture containing M- and p-cresols by treating the initial mixture with urea in an organic solvent, hydrocarbon. fractions. The resulting molecular compound M-cresol and urine are sifted by filtration and subjected to decomposition in water, followed by isolation of the target product by known methods ij. The disadvantage of this method is to carry out the process of decomposition of the molecular compound of urea im-cresol in an aqueous medium, which requires concentration of the solutions of urea so that it can be used again during processing. In addition, the properties of urea during concentration deteriorate due to its decomposition and thus the loss of urea increases. The use of the known method also does not allow obtaining high purity m-cresol. The purpose of the invention is to train m-cresol of high purity .... The goal is achieved by the method of m-cresol recovery from the mixture Keeping m- and p-cresols, by treating the initial mixture with urea in an organic solvent medium, isolating the resulting molecules of the Johny joints of m - cresol and urea by filtration, followed by its decomposition at elevated temperatures in a solvent into m - cresol and m ashesin. As an organic solvent, at the stage of processing the initial mixture with mohevine and as a solvent. At the stage of decomposition of the molecular compound of m-cresol and urea, a solvent selected from the group including benzene, then luol, xylene, ethylbenzene, isopropylbenzene, methylisopropylbenzene, chlorobenzene, diethyl ether, diisopropyl ether, tetrahydrofuran, dioxane, and a man, which is a man is a man from the group. in the temperature range from to the boiling point of the reaction mixture. Example 1. CMeqb 65% of m-crezol and 35% p cresol of aOE kg are mixed with toluene (50 kg) and urea (45 kg) is added to it with simultaneous agitation. The resulting mixture, which is in the form of a suspension, is cooled to a temperature and centrifuged. The resulting filter cake after washing with toluene (20 kg) is cooled to -10 ° C and (150) kg added to toluene. This mixture is stirred at 80 ° C. for 10 minutes and filtered while heating, resulting in the recovery of urea (43 kg). The filtrate is evaporated and distilled, resulting in a pure M-cresol (58 kg). The recovered urea can be reused. The resulting product contains,%: m -cresol 99, water Ofl, impurities 0.4, cresols 995 urea 5. PRI mme R 2. A mixture of 35% M -cresol and 65% L-cresol (100 kg) is mixed with chlorobenzene (10 kg) and urea (1-8 kg) at 50 ° C. The resulting mixture is cooled before and centrifuged. The product obtained is washed with chlorobenzene (7 kg), cooled to 0 ° C and added to chlorobenzene (120 kg). This mixture was stirred at 30 ° C for 1 h and filtered. After distillation, pure M-cresol (18 kg) is crawling. The quality of the product is similar to the example. 1. froze. 100 kg of a mixture of 70% M-cresol, 10% P-cresol, 10% styrene and 10% acetophenone are mixed with isopropyltoluene (30 kg.) Regenerated urea (50 kg) at. The resulting mixture is slowly cooled to within 1 hour of stirring and filtered. The resulting filter cake was washed with isopropyltoluene (30 kg) and added to isopropyltoluene (70 kg). The mixture is heated to 5 minutes and then filtered. The filtrate is evaporated and. distill. 50 kg of the desired product are obtained with a purity as in Example 1. Example 4. Molecular compound W-cresol and urea (16.8 kg) is mixed with toluene (25.2 kg), heated to within 5 minutes. The reaction mixture is filtered under heating and 5.7 kg of urea is obtained. The filtrate is evaporated and distilled to give -cresol (10.5 kg) of purity as in Example 1. P and measures 5. To 36 kg of a mixture of urea and M-cresol and urea molecular compound are added 100 kg of chlorobenzene and the mixture is stirred at 60 ° C within 20 minutes. The reaction mixture is filtered and 25 kg of urea is recovered. The filtrate is evaporated and distilled to give 10.5 kg of pure M - cresol. EXAMPLE 6 To a mixture of 3.6 kg of urea and molecular compound of urea and M-cresol (mass ratio of Leuchin; M-cresol is
3 10537414
3: 7) 15 kg of tetrahydrofuran are added, evaporated and distilled from the wound, and the mixture is stirred to obtain 1.1 kg of m -cresol at room temperature at the same time as in Example 1. 30 min The reaction mixture was decanted, the decantate was decanted, and the remaining mixture was filtered to obtain 2.5% to obtain m-cresol of high-purity. Filtrate and decantation of purity.

权利要求:
Claims (2)
[1]
1. METHOD FOR ISOLATING M-CRESOL FROM A MIXTURE CONTAINING M- AND P> -CERESOLS by treating the initial mixture with urea in an organic solvent medium, isolating the obtained molecular compound of m-cresol and urea by filtration, followed by its decomposition at an elevated temperature in the solvent to us- cresol. and urea, different I. the fact that, in order to obtain high purity M-cresol, an organic solvent is used at the stage of processing the initial mixture with urea and a solvent selected from the group consisting of benzene, toluene, xylene, ethylbenzene, isopropylbenzene, methylisopropylbenzene, chlorobenzene, diethyl ether, diisopropyl ether, tetrahydrofuranμ /. dioxane.
[2]
2. The method of pop. 1, characterized in that the decomposition of the molecular compound M-cresol and urea is carried out in the temperature range from 20 ° C to the boiling point of the reaction mixture.
Priority p o item m, p about signs:
07.22.70 according to claim 1, when using a solvent selected from the group consisting of benzene, toluene, xylene, ethylbenzene, isopropylbenzene, methylisopropylbenzene, chlorobenzene;
12/12/2010 according to claim 1, when using a solvent ^ selected from the group including diethyl ether, diisopropyl ether, tetrahydrofuran, dioxane;
12/08/70 according to claim 2.
SU _(I1 1053741>

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引用文献:

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公开号 | 申请日 | 公开日 | 申请人 | 专利标题

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US1830859A|1927-09-14|1931-11-10|Schering Kahlbaum Ag|Process for separating meta-cresol from phenolic mixtures|

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GB1191631A|1966-05-24|1970-05-13|Struthers Scientific Int Corp|Separation of M-Cresol from Cresol Mixtures|US4044052A|1972-11-03|1977-08-23|Sumitomo Chemical Company, Limited|Process for recovery of urea from its phenolic solution|

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US3998853A|1975-12-04|1976-12-21|Phillips Petroleum Company|13-Oxatetracyclo[8.2.12,9.0.03,8 ]tridec-5-ene-1,5,6,10-tetracarbonitrile|

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US4080327A|1976-07-22|1978-03-21|Phillips Petroleum Company|13-Oxatetracyclo[8.2.12,9.0.03,8 ]tridec-5-ene-1,5,6,10-tetracarbonitrile and separation of its monocyclic aromatic clathrates|

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CN102167658A|2011-03-16|2011-08-31|北京化工大学|Technology for complexing, crystallizing, separating and purifying metacresol|

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CN103333051B|2013-07-18|2015-12-23|北京旭阳化工技术研究院有限公司|A kind of method of producing meta-cresol|

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CN104230669B|2014-09-11|2017-02-08|苏州飞翔新材料研究院有限公司|Separation and purification method of m-cresol|

法律状态:

优先权:

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申请号 | 申请日 | 专利标题

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JP6463670|1970-07-22|

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JP10997970|1970-12-08|

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JP10998070|1970-12-08|

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