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Production method for aromatic polycarbonate resin having increased molecular weight

A polycarbonate resin, high molecular weight technology, applied in the field of aromatic polycarbonate resin manufacturing, can solve the problems such as the inability to increase the molecular weight of polycarbonate, difficulty in removing aromatic monohydroxy compounds, and reduced reaction speed, etc., to achieve thermal good stability effect

Inactive Publication Date: 2015-07-22
MITSUBISHI GAS CHEM CO INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Unlike the interfacial polymerization method, the melt polymerization method has the advantage of not using a solvent, etc., but has the following essential problems: the viscosity of the polymer in the system rises rapidly while the polymerization proceeds, and it is difficult to efficiently remove the aromatics produced as by-products. When the monohydroxyl compound is removed from the system, the reaction rate is significantly reduced, and it is difficult to increase the degree of polymerization
[0008] However, in the methods disclosed in these gazettes, the molecular weight of polycarbonate cannot be sufficiently increased.
If the molecular weight is increased by the method of using a large amount of the above-mentioned catalyst or under severe conditions such as imparting high shear, there will be a problem that the color of the resin will deteriorate or crosslinking reactions will adversely affect the resin.
[0021] The method of increasing the molecular weight of polycarbonate using a linking agent composed of these aliphatic diol compounds can maintain the original good quality of polycarbonate, and can easily and quickly produce polycarbonate with a sufficiently high molecular weight. However, further improvement is expected for the production method of high-molecular-weight polycarbonate resin with better thermal stability

Method used

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  • Production method for aromatic polycarbonate resin having increased molecular weight
  • Production method for aromatic polycarbonate resin having increased molecular weight
  • Production method for aromatic polycarbonate resin having increased molecular weight

Examples

Experimental program
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Effect test

Embodiment

[0198] Hereinafter, the present invention will be described by way of examples, but the present invention is not limited by these examples. However, the measured values ​​in the Examples were measured using the following methods or devices.

[0199] 1) Polystyrene-equivalent weight-average molecular weight (Mw): Using GPC, chloroform was used as a developing solvent, and standard polystyrene (manufactured by Tosoh Corporation, "PStQuick MP-M" with known molecular weight (molecular weight distribution=1) was used. ) to make a standard curve. The dissolution time and molecular weight value of each peak were plotted from the measured standard polystyrene, and the approximate calculation was performed using the cubic formula to prepare a calibration curve. The weight average molecular weight (Mw) was calculated|required by the following calculation formula.

[0200] [calculation formula]

[0201] Mw=Σ(W i × M i )÷Σ(W i )

[0202] Among them, i represents the ith split point...

manufacture example 1

[0245]

[0246] 10,000.6 g (43.808 moles) of 2,2-bis(4-hydroxyphenyl) propane, 10,557 g (49.295 moles) of diphenyl carbonate, and 1.0 μmol / mol-BPA of cesium carbonate as a catalyst (catalyst as relative to 2 , calculated by the number of moles of 2-bis(4-hydroxyphenyl)propane) was put into a 50 L SUS reactor equipped with a stirrer and a distillation device, and the system was replaced with a nitrogen atmosphere. The degree of reduced pressure was adjusted to 27 kPaA (200 torr), the heating medium was set to 205° C., and the raw materials were heated and melted, followed by stirring.

[0247] Then, gradually increase the temperature of the heat medium while reducing the decompression degree, and use the cooling tube to condense and remove the phenol distilled from the reaction system to carry out the transesterification reaction. After about 4 hours, the inside of the system was finally adjusted to 260° C., the degree of reduced pressure was reduced to 0.13 kPaA (1 torr), an...

Embodiment 2

[0253] Put 33.3000 g of the above polycarbonate prepolymer into a 300 cc four-necked flask equipped with a stirrer and a distillation device, and heat and melt at 280°C. Add 0.2840 g (0.001772 mol) of 2-butyl-2-ethyl-propane-1,3-diol as an aliphatic diol compound, add at a jacket temperature of 280°C under normal pressure, and stir and knead for 3 minute. Next, the pressure was adjusted to 0.04 kPaA (0.3 torr) at 280° C., stirred and kneaded for 60 minutes, and a transesterification reaction was performed. Use the cooling tube to distill the phenol, cyclic carbonate (5-butyl-5-ethyl-1,3-dioxan-2-one) and unreacted 2-butyl-2- Ethyl-propane-1,3-diol was coagulated and removed to obtain a cyclic carbonate (5-butyl-5- ethyl-1,3-dioxan-2-one) polycarbonate resin.

[0254] 1 g of the obtained sample resin was put into a test tube, and dried for 2 hours by a cylinder heater set at 120° C. in a glove box (oxygen concentration: 0.0%) substituted with nitrogen. Next, in the same glo...

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Abstract

The present invention provides a method for producing an aromatic polycarbonate resin having increased molecular weight, that not only has excellent quality having high molecular weight and high fluidity, but also has better heat resistance properties. This production method includes a molecular weight increasing step in which an aromatic polycarbonate prepolymer and an aliphatic diol compound having a hydroxymethyl group (HO-CH2-) bonded to a quaternary carbon atom indicated in general formula (I) are reacted in the presence of a transesterification catalyst, and the aromatic polycarbonate resin having increased molecular weight is obtained. (In the formula, Ra-Rf, n, and m are as defined in the Specifications and Claims.)

Description

technical field [0001] The present invention relates to a method for producing a high-molecular-weight aromatic polycarbonate resin. In detail, the present invention relates to a process including a step of reacting an aromatic polycarbonate prepolymer and an aliphatic diol compound of a specific structure to obtain a high-molecular-weight aromatic polycarbonate resin. A method for producing an aromatic polycarbonate resin. Background technique [0002] Since polycarbonate is excellent in heat resistance, impact resistance, and transparency, it is widely used in many fields in recent years. [0003] Many studies have been made conventionally on the production method of this polycarbonate. Among them, polycarbonates derived from aromatic dihydroxy compounds such as 2,2-bis(4-hydroxyphenyl)propane (hereinafter referred to as "bisphenol A") can be obtained by interfacial polymerization or melt polymerization. Manufacturing methods for industrialization. [0004] According t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/42C08G64/04
CPCC08G64/06C08G64/04C08G64/42C08G64/305
Inventor 伊佐早祯则平岛敦原田英文伊藤真树早川淳也矶部刚彦德竹大地新开洋介
Owner MITSUBISHI GAS CHEM CO INC
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