Tert-butyl B'B2-containing triamine monomer, hyperbranched polyimide thereof and preparation method

A technology of triamine monomer and polyimide, which is applied in the field of polyimide, can solve the problems of complex synthesis of type monomers, prone to cross-linking reaction, difficult industrialization, etc., and achieves good solubility, low cost, Avoid gel effects

Active Publication Date: 2016-10-26
上海席亚高分子材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Usually there are two ways to synthesize hyperbranched polyimide, one, first synthesize AB 2 type monomer, and then self-condensation to obtain hyperbranched polyimide, this method can effectively avoid the cross-linking reaction in the polymerization process, but AB 2 The synthesis of B-type monomer is complicated, the cost is high, and it is difficult to industrialize; two, at first synthesize B 3 Type triamine monomer, and then carry out "A 2 +B 3 "The hyperbranched polyimide is obtained by polycondensation. The advantage of this method is that the triamine monomer is relatively easy to synthesize, but cross-linking reactions are very easy to occur during the polycondensation process, so it is difficult to industrialize

Method used

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  • Tert-butyl B'B2-containing triamine monomer, hyperbranched polyimide thereof and preparation method
  • Tert-butyl B'B2-containing triamine monomer, hyperbranched polyimide thereof and preparation method
  • Tert-butyl B'B2-containing triamine monomer, hyperbranched polyimide thereof and preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment one (containing tert-butyl B'B 2 Synthesis of type triamine monomer):

[0038] Preparation of tert-butyl B'B 2 The reaction process of type triamine monomer is as follows:

[0039]

[0040] The following is only a preparation example to specifically illustrate a tert-butyl-containing B'B 2 Type triamine monomer preparation method, those skilled in the art can understand the tert-butyl-containing B'B provided in the present invention on the basis of the following disclosure and in combination with common knowledge in the field 2 The preparation method of type triamine monomer and the various modifications and adjustments of the following preparation methods, so the specific parameters and reagents in the following examples are not used to limit the protection scope of the present invention.

[0041] The present embodiment contains tert-butyl B'B 2 The preparation method of type triamine monomer is as follows: dissolve 100mmol p-tert-butylaniline in 90mL...

Embodiment 2

[0045] Embodiment two (synthesis of HPI-1):

[0046] The polymerization reaction principle for preparing HPI-1 is as follows:

[0047]

[0048] Concrete preparation process is as follows:

[0049] Under nitrogen protection, 1 mmol of the tert-butyl-containing B'B 2 Type triamine monomer 1 was added to a 50mL three-neck round bottom flask, then 15mL DMAc and 1mmol 6FDA were added in sequence, stirred and reacted at room temperature for 4h to obtain a viscous reaction solution, 7mL xylene was added, and the reaction was refluxed for 4h. After the reaction solution was cooled to room temperature, it was slowly poured into 200 mL of rapidly stirred deionized water, and a white powdery solid was precipitated. After suction filtration and air drying, HPI-1 resin was obtained. attached figure 2 is the infrared spectrogram of the polymer film, where 1791cm -1 and 1737cm -1 The absorption peak at is the characteristic absorption peak of the carbonyl group on the imide ring in...

Embodiment 3

[0051] Embodiment three (synthesis of HPI-2):

[0052] The polymerization reaction principle for preparing HPI-2 is as follows:

[0053]

[0054] The specific implementation process is as follows:

[0055] Under the protection of nitrogen, 1 mmol of the triamine monomer 1 was added to a 50 mL three-necked round-bottomed flask, and then 15 mL of DMAc and 1.5 mmol of 6FDA were added in sequence, and the reaction was stirred at room temperature for 4 h to obtain a viscous reaction solution, and 7 mL of xylene was added. Reflux reaction 4h. After the reaction solution was cooled to room temperature, it was slowly poured into 200 mL of rapidly stirred deionized water, and a white powdery solid was precipitated. After suction filtration and air drying, HPI-2 resin was obtained. attached image 3 is the infrared spectrogram of the polymer film, where 1789cm -1 and 1723cm -1 The absorption peak at is the characteristic absorption peak of the carbonyl group on the imide ring i...

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Abstract

The invention discloses tert-butyl B'B2-containing triamine monomer with unequal activation functional groups, hyperbranched polyimide of the tert-butyl B' B2-containing triamine monomer and a preparation method. The triamine monomer is prepared by carrying out three-step reaction including nitrating, substituting and reducing on tert-butylaniline. Based on difference of activities of three amines of the monomer, the monomer and various commercial dianhydride monomers can be used for preparing the hyperbranched polyimide by a 'two-step method', and gel is avoided. The prepared hyperbranched polyimide has good thermal stability and solubility, and has wide application prospect in the fields of gas film separation, high-temperature-resistant polymer processing and the like.

Description

technical field [0001] The invention relates to the technical field of polyimide, in particular to a tert-butyl-containing B'B 2 Type triamine monomer and its hyperbranched polyimide and preparation method. Background technique [0002] Polyimide is a kind of polymer material with excellent heat resistance. Due to its excellent comprehensive performance, it is widely used in various fields such as aviation, aerospace, electrical, machinery, chemical industry, and microelectronics. On the other hand, hyperbranched polymers have unique advantages such as low viscosity and a large number of terminal functional groups. Therefore, the design and development of hyperbranched polyimide is expected to obtain a new material that combines the excellent properties of the above two types of polymers. [0003] Usually there are two ways to synthesize hyperbranched polyimide, one, first synthesize AB 2 type monomer, and then self-condensation to obtain hyperbranched polyimide, this met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C07C211/54C07C209/36
CPCC07C209/10C07C209/36C07C209/76C07C211/54C08G73/10C08G73/1003C08G73/1067C07C211/52C07C211/56
Inventor 伊朗黄卫颜德岳
Owner 上海席亚高分子材料有限公司
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