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Method for synthesizing diphenyl carbonate by employing ionic liquid as accelerant

A technology of diphenyl carbonate and ionic liquid, applied in the field of synthesis of diphenyl carbonate, can solve the problems of strong corrosiveness to industrialization, harsh process conditions, difficult recovery, etc., and achieves high yield, stable process, and reduced The effect of production costs

Inactive Publication Date: 2017-07-25
濮阳市宏源石油化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adoption of AlCl in the mid-1970s 3 , ZnCl 2 Lewis acid is used as a catalyst for transesterification, and the yield is slightly improved, but its strong corrosiveness brings difficulties to industrialization
After the 1980s, metal-organic catalysts such as titanium, aluminum, and tin were developed to increase the yield of diphenyl carbonate (DPC) to more than 30%; among them, the compound of PbO and butyl titanate was used as the transesterification synthesis The catalyzer of DPC, DMC transformation rate 45.4%, the productive rate of DPC, methyl phenyl carbonate (MPC) is respectively 26.3%, 19.1%, the selectivity of DPC is 58.0%, does not have anisole generation; Although titanate High activity, but easy to decompose when encountering water and air, demanding process conditions, and difficult to recycle; organotin has high activity, is not afraid of water and air, but it is easy to pollute the product due to loss, so that the DPC is tinted gray

Method used

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  • Method for synthesizing diphenyl carbonate by employing ionic liquid as accelerant
  • Method for synthesizing diphenyl carbonate by employing ionic liquid as accelerant
  • Method for synthesizing diphenyl carbonate by employing ionic liquid as accelerant

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preparation example Construction

[0033] Preferably, the preparation method of the first catalyst comprises: uniformly mixing the ionic liquid and the metal organic matter, adding an ethanol solution of neodymium nitrate and stirring uniformly, and then heating to remove the ethanol to obtain the first catalyst; wherein, the neodymium nitrate accounts for 3% of the mass of the ethanol solution. %~5%, the molar ratio of neodymium nitrate to ionic liquid is (0.05~0.1):1.

[0034] Describe below in conjunction with specific implementation manner:

Embodiment 1

[0036] The invention provides a kind of method taking ionic liquid as promotor synthetic diphenyl carbonate, it is characterized in that, comprises the following steps:

[0037] S101: Carrying out a pressurized reaction rectification process of phenol and dimethyl carbonate under the action of the first catalyst, after the transesterification reaction, to benzyl carbonate and methanol; wherein, the feeding ratio of dimethyl carbonate and phenol is 0.9, The first catalyst comprises an ionic liquid [C 2 mim][PF 4 ]-H 2 SO 4 and [N 2222 ][PF 4 ]-TFSA, organometallic Ti(OBu) 4 , [C 2 mim][PF 4 ]-H 2 SO 4 , [N 2222 ][PF 4 ]-TFSA and Ti(OBu) 4 The molar ratio is 0.25:0.25:1, and the addition of the first catalyst is 0.5wt% of the total mass of phenol and dimethyl carbonate, the pressure of the pressurized reaction rectification process is 2.5MPa, the temperature is 215 ° C, and the time is 3h.

[0038] S102: The benzyl carbonate obtained in S101 is subjected to a dispr...

Embodiment 2

[0045] The invention provides a kind of method taking ionic liquid as promotor synthetic diphenyl carbonate, it is characterized in that, comprises the following steps:

[0046] S101: Carrying out a pressurized reaction rectification process of phenol and dimethyl carbonate under the action of the first catalyst, after the transesterification reaction to benzyl carbonate and methanol; wherein, the feeding ratio of dimethyl carbonate and phenol is 0.6, The first catalyst comprises an ionic liquid [C 4 mim][BF 4 ]-H 2 SO 4 and [N 2222 ][NTf 2 ]-TFSA, Metalorganic Bu 2 SnO, [C 4 mim][BF 4 ]-H 2 SO 4 , [N 2222 ][NTf 2 ] - TFSA and Bu 2 The molar ratio of SnO is 0.005:0.005:1, and the addition amount of the first catalyst is 2wt% of the total mass of phenol and dimethyl carbonate, the pressure of the pressurized reaction rectification process is 0.55MPa, the temperature is 230°C, and the time is 1h.

[0047] S102: The benzyl carbonate obtained in S101 is subjected to ...

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Abstract

The invention relates to a method for synthesizing diphenyl carbonate by employing an ionic liquid as an accelerant. According to the method, the ionic liquid is adopted as a catalytic phenol and is exchanged with dimethyl carbonate to synthesize an accelerant of a diphenyl carbonate metal organic matter catalyst. Through the synergistic effect of the ionic liquid and a metal organic matter, separation of dimethyl carbonate and methyl alcohol is significantly improved, the catalytic activity of the metal organic matter is improved and the yield of diphenyl carbonate DPC and methyl phenyl carbonate MPC is improved, wherein the conversion rate of DMC is greater than 50% and the yield of DPC is greater than 80%; and the energy consumption of the method is lower. According to the method, generation of a by-product anisole in transesterification of DMC and phenol is inhibited to a great extent; and an azeotropic composition of DMC and methyl alcohol is changed and methyl alcohol is more easily separated from a reaction system, so that the yield of DPC and MPC is significantly improved.

Description

technical field [0001] The invention relates to the technical field of synthesis of diphenyl carbonate, in particular to a method for synthesizing diphenyl carbonate with an ionic liquid as an accelerator. Background technique [0002] As an important chemical intermediate, diphenyl carbonate can be used to synthesize many important organic compounds and polymer materials, especially it can replace highly toxic phosgene and bisphenol A to produce polycarbonate with excellent performance. There are three main synthetic methods of diphenyl carbonate: phosgene method, transesterification method and oxidative carbonylation method. Due to the use of highly toxic and highly corrosive phosgene, the phosgene method has seriously polluted the environment and has been gradually eliminated; although the oxidative carbonylation method has a high atom utilization rate, the catalyst used is expensive and has poor catalytic performance. High, therefore, do not see the report of industrial...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/06C07C69/96
CPCC07C68/06C07C69/96
Inventor 王际东周志茂屈一新武胜强
Owner 濮阳市宏源石油化工有限公司