CN102531908B - The preparation method of methyl benzol carbonate - Google Patents
The preparation method of methyl benzol carbonate Download PDFInfo
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- CN102531908B CN102531908B CN201110449387.5A CN201110449387A CN102531908B CN 102531908 B CN102531908 B CN 102531908B CN 201110449387 A CN201110449387 A CN 201110449387A CN 102531908 B CN102531908 B CN 102531908B
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Abstract
The present invention relates to a kind of method preparing methyl benzol carbonate, with methylcarbonate and diphenyl carbonate for raw materials, put into diphenyl carbonate and catalyzer in rectification and purification reactor after, material is slowly warming up to 130 DEG C ~ 180 DEG C, then in reactor, slowly methylcarbonate is added dropwise to by the rate of addition of 0.5 ~ 15ml/min, maintain afterwards reacting liquid temperature time 1 ~ hour, again by reactor vacuum degree control at-0.07 ~-0.099Mpa, slow raising reacting liquid temperature to 180 DEG C ~ 240 DEG C carries out rectification and purification, the cut collected at this temperature is product methyl benzol carbonate.The present invention effectively can solve the use severe toxicity raw material existed in prior art, the problem such as resultant of reaction is poisonous, product yield is not high and purification process is difficult.
Description
Technical field
The invention belongs to the preparing technical field of fine chemical product, relate to a kind of method preparing methyl benzol carbonate.
Background technology
Methyl benzol carbonate is the intermediate product that phenol and methylcarbonate ester exchange synthesizing diphenyl carbonate react, disproportionation reaction Formed diphenyl phthalate and methylcarbonate can be there is in self, so the yield important to ester-interchange method diphenyl carbonate synthesis, and it is also an important indicator of methylcarbonate transformation efficiency.
It is generate methyl benzol carbonate with phenyl chloroformate and methyl alcohol reaction that the processing method that methyl benzol carbonate is prepared in current this area mainly contains two kinds: one, the shortcoming of this technique is: the phenyl chloroformate employing severe toxicity is raw material, also containing toxic substance methylene dichloride in resultant, and reacted product needs could obtain the higher methyl benzol carbonate of purity after the washing of multiple working procedure, drying and purification.Another kind of processing method uses phenol and methylcarbonate to carry out transesterification reaction to generate methyl benzol carbonate, the shortcoming of this technique is: react wayward, methyl benzol carbonate is easy to disproportionation Formed diphenyl phthalate, and the yield of methyl benzol carbonate is very low, reacted product needs just can obtain the methyl benzol carbonate that purity is 98% after multi step strategy.In addition to the above methods, the research report of p-methylphenyl carbonic ether is less both at home and abroad at present, market does not have yet highly purified methyl benzol carbonate product sell, this present situation hinders the analysis and research work of ester exchange synthesizing diphenyl carbonate to a great extent, therefore carries out the highly purified methyl benzol carbonate technical study important in inhibiting of preparation.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of methyl benzol carbonate, to solve the use severe toxicity raw material existed in prior art, the problem such as resultant of reaction is poisonous, product yield is not high and purification process is difficult.
For realize the technical solution of foregoing invention object be adopt mass ratio be 1: 1 ~ 5 methylcarbonate and diphenyl carbonate as raw materials, and to be prepared by following processing step:
The first step, puts into diphenyl carbonate and catalyzer successively by the mass ratio of 100: 0.5 ~ 10, mixes in rectification and purification reactor, and catalyzer used is Lewis acid, metal oxide, titanate or organic tin catalyzer;
Second step, is slowly warming up to 130 DEG C ~ 180 DEG C by the mixture through above step, then in reactor, be slowly added dropwise to methylcarbonate by the rate of addition of 0.5 ~ 15ml/min;
3rd step, after methylcarbonate dropwises, maintain reacting liquid temperature, the time is 1 ~ 10 hour;
4th step, opens vacuum system, and by reactor vacuum degree control at-0.07 ~-0.099Mpa, slowly improve reacting liquid temperature to 180 DEG C ~ 240 DEG C and carry out rectification and purification, the cut collected at this temperature is product methyl benzol carbonate.
In the technology of the present invention solution, the preferred value of the methylcarbonate added in rectification and purification reactor and the mass ratio of diphenyl carbonate is 1: 3; The preferred value of the mass ratio of catalyzer and diphenyl carbonate is 3: 100.
In the technology of the present invention solution, the preferred substance of used catalyst is lead phenolate or tetrabutyl titanate or Dibutyltin oxide.
Preferred version of the present invention, put into diphenyl carbonate and catalyst mix material in rectification and purification reactor after, is slowly warming up to 150 DEG C, then in reactor, is slowly added dropwise to methylcarbonate by the rate of addition of 1.5ml/min; Maintain 8 hours reacting liquid temperature time afterwards, then by reactor vacuum degree control at-0.098Mpa, slowly improve reacting liquid temperature to 205 DEG C and carry out rectification and purification, the cut collected at this temperature is product methyl benzol carbonate.
Compared with prior art, the beneficial effect that the present invention has is;
One, use that advantages of nontoxic raw materials---the present invention uses methylcarbonate and diphenyl carbonate to be raw material, avoid prior art and use hypertoxic raw material phenyl chloroformate and the safety brought and problem of environmental pollution.
Two, preparing product purity is high---and the methyl benzol carbonate purity that the present invention is preferably prepared can reach 99.9%, and the methyl benzol carbonate purity that than ever prepared by technique all wants high.
Three, preparation technology is simple---and the present invention only needs reaction and the rectification and purification process that can complete methyl benzol carbonate in set of device (rectification and purification reactor), do not need, again through processing steps such as washing, dryings, to enormously simplify technological process.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but protection scope of the present invention is not limited to following embodiment.
Embodiment one
Get 200g diphenyl carbonate and 4g tetrabutyl titanate adds in reactor, after progressively raising reacting liquid temperature to 140 DEG C, be slowly added dropwise to methylcarbonate 140g, rate of addition is 1ml/min; After methylcarbonate dropwises, maintain reacting liquid temperature 3 hours; Open vacuum system, reacting liquid temperature, at-0.085Mpa, is slowly increased to 220 DEG C and carries out rectification and purification, collect the cut at this temperature by reactor vacuum degree control, and obtaining purity is the methyl benzol carbonate of 99.91%.
Embodiment two
Get 200g diphenyl carbonate and 2g Dibutyltin oxide adds in reactor, after progressively raising reacting liquid temperature to 170 DEG C, be slowly added dropwise to methylcarbonate 300g, rate of addition is 5ml/min; After methylcarbonate dropwises, maintain reacting liquid temperature 5 hours.Open vacuum system, reacting liquid temperature, at-0.095Mpa, is slowly increased to 210 DEG C and carries out rectification and purification, collect the cut at this temperature by reactor vacuum degree control, and obtaining purity is the methyl benzol carbonate of 99.93%.
Embodiment three
Get 200g diphenyl carbonate and 8g lead phenolate adds in reactor, after progressively raising reacting liquid temperature to 150 DEG C, be slowly added dropwise to methylcarbonate 270g, rate of addition is 1.5ml/min; After methylcarbonate dropwises, maintain reacting liquid temperature 8 hours.Open vacuum system, reacting liquid temperature, at-0.098Mpa, is slowly increased to 205 DEG C and carries out rectification and purification, collect the cut at this temperature by reactor vacuum degree control, and obtaining purity is the methyl benzol carbonate of 99.95%.
Claims (3)
1. a preparation method for methyl benzol carbonate, is characterized in that: get 200g diphenyl carbonate and 4g tetrabutyl titanate adds in reactor, and after progressively raising reacting liquid temperature to 140 DEG C, be slowly added dropwise to methylcarbonate 140g, rate of addition is 1ml/min; After methylcarbonate dropwises, maintain reacting liquid temperature 3 hours; Open vacuum system, reacting liquid temperature, at-0.085Mpa, is slowly increased to 220 DEG C and carries out rectification and purification, collect the cut at this temperature by reactor vacuum degree control, and obtaining purity is the methyl benzol carbonate of 99.91%.
2. the preparation method of a methyl benzol carbonate, it is characterized in that: get 200g diphenyl carbonate and 2g Dibutyltin oxide adds in reactor, after progressively raising reacting liquid temperature to 170 DEG C, be slowly added dropwise to methylcarbonate 300g, rate of addition is 5ml/min; After methylcarbonate dropwises, maintain reacting liquid temperature 5 hours; Open vacuum system, reacting liquid temperature, at-0.095Mpa, is slowly increased to 210 DEG C and carries out rectification and purification, collect the cut at this temperature by reactor vacuum degree control, and obtaining purity is the methyl benzol carbonate of 99.93%.
3. a preparation method for methyl benzol carbonate, is characterized in that: get 200g diphenyl carbonate and 8g lead phenolate adds in reactor, and after progressively raising reacting liquid temperature to 150 DEG C, be slowly added dropwise to methylcarbonate 270g, rate of addition is 1.5ml/min; After methylcarbonate dropwises, maintain reacting liquid temperature 8 hours; Open vacuum system, reacting liquid temperature, at-0.098Mpa, is slowly increased to 205 DEG C and carries out rectification and purification, collect the cut at this temperature by reactor vacuum degree control, and obtaining purity is the methyl benzol carbonate of 99.95%.
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| CN103467283B (en) * | 2013-09-29 | 2015-06-10 | 陕西省石油化工研究设计院 | Method for using double towers to ceaselessly compound high-purity methyl phenyl carbonic ester |
| CN109433183B (en) * | 2018-11-01 | 2021-09-03 | 河南科技学院 | Bimetal composite oxide catalyst, preparation method and application |
| CN114931975B (en) * | 2022-04-13 | 2023-07-07 | 河南科技学院 | Catalyst for synthesizing diphenyl carbonate, preparation method and application of diphenyl carbonate |
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| JPH0791234B2 (en) * | 1990-12-26 | 1995-10-04 | 旭化成工業株式会社 | Continuous production of aromatic carbonates |
| JPH10139736A (en) * | 1996-11-12 | 1998-05-26 | Mitsubishi Chem Corp | Production of alkyl aryl carbonate |
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| 高纯度甲基苯基碳酸醋的制备及其定量分析;邢爱华等;《中国化学会全国微波化学学术研讨会论文摘要集》;20051001;135-139 * |
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Address after: No.61 Xiyan Road, Yanta District, Xi'an City, Shaanxi Province, 710054 Patentee after: Shaanxi Chemical Research Institute Co.,Ltd. Address before: No.61 Xiyan Road, Xi'an City, Shaanxi Province 710054 Patentee before: SHAANXI RESEARCH DESIGN INSTITUTE OF PETROLEUM CHEMICAL INDUSTRY |
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