Biphenyltetracarboxylic acid dianhydride, method for producing the same, polyimide using the same and method for producing the same

A technology of biphenyltetracarboxylic dianhydride and biphenyltetracarboxylic acid, applied in the field of biphenyltetracarboxylic dianhydride and its manufacture, achieving high productivity, excellent heat resistance, and high degree of polymerization

Active Publication Date: 2007-06-06
MITSUBISHI RAYON CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, as described in the examples of USP4958002, although the high-purity BPDA with a ternary derivative content of 0.06%

Method used

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  • Biphenyltetracarboxylic acid dianhydride, method for producing the same, polyimide using the same and method for producing the same
  • Biphenyltetracarboxylic acid dianhydride, method for producing the same, polyimide using the same and method for producing the same
  • Biphenyltetracarboxylic acid dianhydride, method for producing the same, polyimide using the same and method for producing the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0115] Use the heater (1) shown in Figures 1 to 4 as the heater (1) shown in Figs. A hollow rotating shaft (3) with a plurality of hollow rotating heating bodies (2) is hidden, and the heated heating medium is transported to the hollow part (20) of the rotating heating body through the hollow part (30) of the rotating shaft ), in addition also to the heating jacket (5), thereby, through the heat transfer from each surface of these rotating shafts, the rotating heating body and the heating jacket arranged as needed, the heat necessary for the reaction can be supplied. The hollow rotating heating body (2) in the heating device has a wedge-shaped shape when viewed from the side, and a roughly fan-shaped shape when viewed from the front, and is fixed to the hollow rotating shaft (3) with the shaft portion of the fan.

[0116] BTC (moisture is 18.31%) is continuously supplied to the above-mentioned heating device from the inlet (41) of the raw material at a ratio of 7.8kg / hour,...

Embodiment 2

[0121] Using the same apparatus as in Example 1, the heat treatment of BTC was performed by continuous operation. BTC (moisture is 18.31%) is continuously supplied by the raw material inlet (41) of the device with the ratio of 7.4kg / hour, and the residence time in the device is to carry out the dehydration reaction under the conditions of 7.7 hours and normal pressure, by the outlet of the product ( 42) Continuous discharge of BPDA. And, during operation, nitrogen gas was introduced from the inlet (61) at a rate of 70 L / min and discharged from the outlet (62). In addition, by adjusting the temperature and flow rate of the heating medium, the heat necessary for the reaction is supplied to achieve the prescribed operating conditions. The heat treatment conditions of the raw materials are shown in Table 2.

[0122] temperature(°C)

time (hours)

Heating rate (℃ / hour)

20→110

0.5

180

110→176

0.5

132

176→210

...

Embodiment 3

[0130] Using the same apparatus as in Example 1, the heat treatment of BTC was performed by batch operation.

[0131] 35kg of BTC (moisture content: 18.31%) was added to the device in advance from the raw material inlet (41). The heat treatment conditions of the raw materials are shown in Table 3.

[0132] In addition, the temperature rise of the BTC is carried out by increasing the temperature of the heating medium supplied to the sleeve (5), but the movement of the BTC is not carried out during the temperature rise (in the following examples / comparative examples, unless otherwise specified, is the same as this).

[0133] temperature(°C)

Example 3

Example 4

Example 5

time (hours)

Heating rate

(℃ / hour)

time (hours)

Heating rate

(℃ / hour)

time (hours)

Heating rate

(℃ / hour)

60→100

0.5

80

2.0

20

0.5

80

100→180

0.5...

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PUM

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Abstract

A process for producing BPDA by which high productivity is attained while maintaining a high purity. The process for biphenyltetracarboxylic acid dianhydride production comprises heating biphenyltetracarboxylic acid to produce biphenyltetracarboxylic acid dianhydride, wherein the heat treatment is conducted at a pressure of 1*102-1.1*105 Pa to a maximum temperature in the range of 210-250 DEG C in such a manner that at least 1/4 the period used for heating from 60 DEG C to 210 DEG C has a heating rate of 50 DEG C/Hr or higher and that the acid is held at 150-250 DEG C for 0.5-10 hours.

Description

technical field [0001] The present invention relates to biphenyltetracarboxylic aciddianhydride (biphenyltetracarboxylic aciddianhydride, hereinafter referred to as BPDA) and its manufacturing method, polyimide using the biphenyltetracarboxylic dianhydride, and its manufacturing method. Background technique [0002] BPDA is a useful compound as a raw material for producing aromatic polyimides, which are currently attracting attention as heat-resistant resins. The method of utilizing BPDA to manufacture aromatic polyimides can be any one of the following methods: the method of making by the polymerization reaction of BPDA and aromatic diamines, the method of making BPDA and aromatic diamines near normal temperature A method of ring-closing imidization of polyamic acid (polyamic acid) obtained by polymerization at low temperature. [0003] BPDA can be obtained by heating biphenyltetracarboxylic acid (hereinafter referred to as BTC) to 100° C. to 500° C. under a reduced pressu...

Claims

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Application Information

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IPC IPC(8): C07D307/89C08G73/10
CPCC07D307/89C08G73/1007C08G73/10C07C63/331C07D407/04
Inventor 三上洋新田诚野口直树
Owner MITSUBISHI RAYON CO LTD
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