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Preparation of high intrinsic viscosity poly(arylene ether) resins

A technology of intrinsic viscosity and polyarylene ether, applied in the direction of one-component polyether rayon, etc., can solve the problem of no preparation and so on

Inactive Publication Date: 2004-01-14
SHPP GLOBAL TECH BV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no guidance for preparing poly(2,6-dimethylphenylene ether) in this molecular weight range

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047]This example provides a method for preparing polyarylether with high intrinsic viscosity, which is based on the results of several practical experiments. 2,6-Xylenol (200 kg) was dissolved in toluene (23660 kg) in a reaction vessel. In xylenol solution, add the solution of cuprous bromide in 48% by weight of HBr aqueous solution (the solution of 105Kg has 6.5% by weight of copper), N, N'-dibutylethylenediamine (DBEDA, 125Kg about 25- 28% by weight in toluene), dimethylbutylamine (DMBA; 237Kg), and di-n-butylamine (DBA; 80Kg). The reaction was carried out in a semi-batch process, continuously adding 2,6-xylenol in 45 minutes and at 175 standard cubic meters per hour (Nm 3 Oxygen is added at a rate of / hr). The oxygen addition rate is based on control of the oxygen concentration. The reaction temperature was initially about 30°C and increased to about 45°C after the exotherm of the reaction. After about 100-120 minutes, when the reading of the embedded viscometer reach...

Embodiment 2-4

[0052] Example 2

Embodiment 5 and 6

[0054] Modify the general steps of Example 1, prolong the reaction time until the intrinsic viscosity of the product no longer increases, and study the influence of the content of the chain terminator in the starting material 2,6-dimethylphenol on the intrinsic viscosity of the product. When 2,6-xylenol contained a total of 0.071% by weight of chain-terminating compounds (measured as 0.062% by weight of p-cresol and 0.009% by weight of 2,4-xylenol), the obtained after prolonged reaction time The intrinsic viscosity of polyarylether is 1.80dL / g. In contrast, when the chain terminator content was limited to 0.035% by weight of the starting 2,6-xylenol, the extended reaction time resulted in a polyarylene ether with an intrinsic viscosity of 2.10 dL / g. This example shows the importance of using a phenol with a small amount of chain terminator in order to obtain a high intrinsic viscosity product.

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PUM

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Abstract

A poly(aryl ether) resin having an intrinsic viscosity greater than about 0.8 dL / g obtained by reacting phenol with oxygen in the presence of an organic solvent and a metal complex catalyst. The concentration of phenol is about 5-15% by weight of the total amount of phenol and solvent, and the molar ratio of metal to phenol in the metal complex catalyst is about 1:100 to 1:200.

Description

Background of the invention: [0001] The invention relates to a method for preparing poly(aryl ether) resin. In particular, the invention relates to a method of preparing high intrinsic viscosity poly(aryl ether) resins. [0002] Commercially available poly(aryl ether) resins typically have number average molecular weights of about 7000-30000 and intrinsic viscosities of about 0.25-0.60 deciliters per gram (dL / g) as measured in chloroform at 25°C. Although high molecular weight is associated with high intrinsic viscosity, there is no simple conversion in the measurement of the two due to the complex dependence of intrinsic viscosity on the specific molecular weight distribution in the sample. The preparation of poly(aryl ether) resins, including some high intrinsic viscosity resins, is described in US Patent 3,219,625 to Blanchard et al. These references generally describe the preparation of poly(phenylene ether) resins using copper catalysts and halide, methoxy and pyridine ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/44C08G65/46D01F6/66
CPCC08G65/46C08G65/44
Inventor A·J·F·M·布拉尔特H·G·E·因格尔布雷希特
Owner SHPP GLOBAL TECH BV
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