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Method and device for recovering solvent used in polyphenyl ether synthesis

A technology of polyphenylene ether and mixed solvents, which is applied in chemical instruments and methods, preparation of organic compounds, separation/purification of hydroxyl compounds, etc. It can solve the problems of content fluctuations due to extraction effects, high energy consumption of rectification, etc.

Pending Publication Date: 2020-06-02
BLUESTAR BEIJING TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a result, methanol obtained after separation still contains toluene, a non-polar solvent, with a content of more than 3%, and the content often fluctuates due to the effect of extraction
[0008] In addition, in the prior art, polar solvents are usually separated by rectification, but rectification consumes a lot of energy. If the energy consumption is to be reduced, the rectification process needs to be further improved

Method used

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  • Method and device for recovering solvent used in polyphenyl ether synthesis
  • Method and device for recovering solvent used in polyphenyl ether synthesis
  • Method and device for recovering solvent used in polyphenyl ether synthesis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0089] The solvent from the solvent recovery tank, which contains 16% toluene, 80% methanol, 3.6% water, 0.39% oligomers, and 0.01% solid particles, enters the filter 1 with a flow rate of 1000Kg / h; the filtered solvent is sent to flash evaporation Tower 2, operating pressure 24KPa (G), operating temperature 72 ℃; From the mixture containing oligomers at the bottom of the flash tower 2, it is delivered to the concentrated distiller with 100Kg / h flow rate, and the concentrated distiller operating pressure is 25KPa (G), The operating temperature is 113°C; the gas phase of the flash tower and the concentrated distiller enters the rectifying tower 4, the operating pressure is 5KPa (G), and the operating temperature is 70°C; Water is mixed into the phase separator, wherein the mass ratio of the amount of water to the methanol in the mixed solvent is 1.3:1; the operating temperature of the phase separator is 30°C, the residence time is 2 hours, and the light phase toluene is extracte...

Embodiment 2

[0091] The solvent from the solvent recovery tank, which contains 19.3% toluene, 77.6% methanol, 2.62% water, 0.47% oligomers, and 0.01% solid particles, enters filter 1 with a flow rate of 1100kg / h; the filtered solvent is sent to flash evaporation Tower 2, operating pressure 22KPa (G), operating temperature 68 ℃; From the mixture containing oligomer at the bottom of the flash tower 2, it is delivered to the concentrated distiller with 112Kg / h flow rate, and the concentrated distiller operating pressure is 23KPa (G), The operating temperature is 110°C; the gas phase of the flash tower and the concentrated distiller enters the rectifying tower 4, the operating pressure is normal pressure 5KPa (G), and the operating temperature is 70°C; The water in the tank is mixed into the phase separator, wherein, the mass ratio of the amount of water to the methanol in the mixed solvent is 1.2:1; the operating temperature of the phase separator is 28°C, the residence time is 2 hours, and th...

Embodiment 3

[0096] Embodiment 3 first high-pressure rectification tower feeds, then normal pressure rectification tower separates

[0097] Solvent composition and feed flow rate are the same as in Example 1, except that the aqueous methanol solution at the bottom of the azeotropic tower 6 first enters the high-pressure rectification tower for separation, and then the material in the high-pressure rectification tower tank enters the atmospheric rectification tower for further separation. The operating pressure of the high-pressure rectification tower is 0.41MPa(G), the temperature of the bottom of the tower is 126°C, and about 50% of methanol is withdrawn from the top of the high-pressure tower with a purity of 99.8%. The operating pressure of the atmospheric tower is 4Kpa (G), and the operating temperature of the tower kettle is 100°C. Methanol is separated from the top of the atmospheric distillation tower with a purity of 99.9%, and the water is discharged from the tower kettle for recyc...

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Abstract

The invention relates to a method and a device for recovering a solvent used in a polyphenyl ether synthesis process. According to the method, the operation of azeotropic distillation of a small amount of toluene in an aqueous phase after extraction separation by using an azeotropic tower is added after conventional extraction separation operation, and a double-tower mode of combination of a normal-pressure separation tower and a high-pressure separation tower is used when methanol in the aqueous phase is recovered. According to the invention, the toluene recovered by the method has improved purity, and can be recycled as a polyphenyl ether synthetic solvent, the recovered methanol has improved purity, and can be recycled as a polyphenyl ether cleaning solvent, and the recovered water hasimproved purity, can be recycled as an extractant, and greatly reduces the energy consumption of the recovered solvent.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for recovering solvent used in polyphenylene ether synthesis and a device thereof. Background technique [0002] Polyphenylene ether can be obtained by polymerizing phenolic compounds in a non-polar solvent or a mixed solvent of polar and non-polar in the presence of oxygen, using an oxidative coupling polymerization catalyst containing copper, manganese or cobalt. The polymerization reaction is terminated and the catalyst is separated, and the obtained polyphenylene ether solution is added into a solvent of poorly soluble polyphenylene ether to precipitate the polyphenylene ether. The precipitated polyphenylene ether is separated from solid and liquid, washed with a polar solvent, and dried to obtain polyphenylene ether powder. Non-polar solvents are usually aromatic hydrocarbon solvents, which are easily soluble solvents for polyphenylene ether, and toluene is commonl...

Claims

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Application Information

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IPC IPC(8): C07C29/76C07C29/82C07C29/86C07C29/80C07C31/04C07C7/00C07C7/04C07C7/06C07C7/10C07C15/06
CPCC07C29/76C07C29/82C07C29/86C07C29/80C07C7/005C07C7/04C07C7/06C07C7/10C07C31/04C07C15/06
Inventor 李振刚王志方丹尼尔彭斌
Owner BLUESTAR BEIJING TECH CENT