Application and preparation method of photocurable polyimide ink for 3D printing

A polyimide and 3D printing technology, applied in the field of 3D printing, can solve the problems of loss of high-strength and high-temperature performance of polyimide, lower fidelity of printed products, low thermal expansion coefficient, etc., and achieve superior shape memory performance, good mechanical The effect of intensity

Active Publication Date: 2019-03-19
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Polyimide-based shape memory materials have been widely studied due to their high mechanical strength, high modulus, low thermal expansion coefficient, and excellent thermal stability. The 3D printing of thermosetting polyimide materials is One of the problems faced is that the printed product will not only shrink in size during post-processing, reducing the fidelity of the printed product, but also lose the original high-strength and high-temperature properties of polyimide
However, there are no reports on 3D printing polyimide inks with shape memory properties.

Method used

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  • Application and preparation method of photocurable polyimide ink for 3D printing
  • Application and preparation method of photocurable polyimide ink for 3D printing
  • Application and preparation method of photocurable polyimide ink for 3D printing

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Embodiment 1

[0032] Embodiment 1 A kind of preparation method of photocurable polyimide ink for 3D printing, comprises the following steps:

[0033] ⑴Preparation of copolymerized polyimide:

[0034] Under nitrogen atmosphere, add N-methyl-2-pyrrolidone (28mL) to 3,5-diaminobenzoic acid (5mmol, 0.746g) and stir until 3,5-diaminobenzoic acid is completely dissolved; then slowly add 4 , 4'-(4,4'-isopropyldiphenoxy) diphthalic anhydride (10mmol, 5.2g), continuously stirred in an ice bath for 20~30h to obtain a mixed solution, which was added with 4,4 'Diaminodiphenyl ether (5mmol, 1.001g) was continuously stirred for 20~30 h to obtain a black polyamic acid solution; the black polyamic acid solution was heated to 240~290°C and stirred for 2~5 h for imidization reaction, In this process, the water molecules produced are removed by a water separator, and finally a black viscous copolyimide solution is obtained. The copolyimide solution is precipitated with absolute ethanol, washed repeatedly with ...

Embodiment 2

[0039] Embodiment 2 A kind of preparation method of photocurable polyimide ink for 3D printing, comprises the following steps:

[0040] (1) Preparation of copolyimide is the same as in Example 1.

[0041] (2) The polyimide grafted with methacrylate is prepared with embodiment 1.

[0042] (3) Preparation of photocurable polyimide ink:

[0043] Dissolve acrylate-grafted polyimide (20wt%) into N-vinyl-2-pyrrolidone (78wt%), then add inhibitor hydroquinone (0.1wt%), photoinitiator Irgacure 2100 (1.9wt%) and stirred for 10 minutes to obtain 3D printed shape memory polyimide ink.

Embodiment 3

[0044] Embodiment 3 A kind of preparation method of photocurable polyimide ink for 3D printing, comprises the following steps:

[0045] (1) Preparation of copolyimide is the same as in Example 1.

[0046] (2) The polyimide grafted with methacrylate is prepared with embodiment 1.

[0047] (3) Preparation of photocurable polyimide ink:

[0048] Dissolve acrylate-grafted polyimide (20wt%) into N-vinyl-2-pyrrolidone (74wt%), and then add the cross-linking monomer isobornyl methacrylate (4wt%), polymerization inhibitor Agent hydroquinone (0.1wt%) and photoinitiator Irgacure 2100 (1.9wt%) were stirred for 25 minutes to obtain 3D printed shape memory polyimide ink.

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Abstract

The invention relates to a preparation method of photocurable polyimide ink for 3D printing. The method includes steps: (1) sequentially adding N-methyl-2-pyrrolidone, 4, 4'-(4,4'-isopropyl diphenoxyl)diphthalic anhydride and 4,4' diaminodiphenyl ether into 3,5-diaminobenzoic acid to obtain copolyimide through imidization; (2) preparing methacrylate grafted polyimide, to be more specific, adding N-methyl-2-pyrrolidone into a copolyimide product to obtain solution A, adding methylacrylic acid-beta-hydroxyethyl ester, N,N'-dicyclohexyl carbimide and 4-dimethylamino pyridine into N-methyl-2-pyrrolidone to obtain solution B, and subjecting the solution A and the solution B to Steglich esterification reaction to obtain methacrylate grafted polyimide; (3) dissolving methacrylate grafted polyimide into N-vinyl-2-pyrrolidone, and sequentially adding isobornyl methacrylate, hydroquinone and Irgacure2100 to obtain photocurable polyimide ink. The invention further discloses application of the ink. The method is simple, and the obtained ink has a shape memory effect and is available for quick photocuring.

Description

technical field [0001] The invention relates to the field of 3D printing, in particular to a preparation method and application of photocurable polyimide ink for 3D printing. Background technique [0002] Shape memory materials (shape memory materials, SMMs) can change their shape according to external stimuli. They are a typical smart material. Shape memory materials include shape memory ceramics, shape memory metals, and shape memory polymers. Shape memory polymers (SMPs) are shape memory materials based on the conformational transformation of polymer chains, which can spontaneously transform from temporary shape to permanent shape under the action of certain external stimuli, and its crystallization / melting transition (or Glass transition) acts as a reversible phase to respond to stimuli, while the cross-linked network acts as a stationary phase to provide resilience, which has the characteristics of large deformation recovery rate, significant shape memory effect, and go...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08F283/04C08F220/18C08F226/10C08J5/18B33Y70/00
CPCB33Y70/00C08F283/045C08G73/1007C08G73/1071C08J5/18C08J2351/08C08F220/1811
Inventor 张新瑞李霄杨增辉王齐华王廷梅
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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