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CN-122011457-A - Transparent shape memory polyimide film and preparation method thereof

CN122011457ACN 122011457 ACN122011457 ACN 122011457ACN-122011457-A

Abstract

The invention provides a transparent shape memory polyimide film and a preparation method thereof, and relates to the technical field of optical films, wherein the preparation method of the transparent shape memory polyimide film comprises the steps of uniformly mixing a mixed diamine monomer, a dianhydride monomer and a first high-boiling-point polar aprotic solvent in a protective gas atmosphere, and carrying out a first stirring reaction to obtain a polyamic acid solution; the mixed diamine monomer comprises 1, 12-diaminododecane and 1, 3-bis (3-aminophenoxy) benzene, the dianhydride monomer comprises bisphenol A type diether dianhydride, and the polyamide acid solution is used for film forming to obtain a polyimide film. The polyimide film prepared by the method has better transparency, better shape memory performance and lower glass transition temperature.

Inventors

  • LIU YANJU
  • JIANG SHUTING
  • KONG DEYAN
  • LENG JINSONG
  • XIAO XINLI

Assignees

  • 哈尔滨工业大学

Dates

Publication Date
20260512
Application Date
20260401

Claims (10)

  1. 1. The preparation method of the transparent shape memory polyimide film is characterized by comprising the following steps: step S1, uniformly mixing a mixed diamine monomer, a dianhydride monomer and a first high-boiling-point polar aprotic solvent in a protective gas atmosphere, and performing a first stirring reaction to obtain a polyamic acid solution, wherein the mixed diamine monomer comprises 1, 12-diaminododecane and 1, 3-bis (3-aminophenoxy) benzene, and the dianhydride monomer comprises bisphenol A type diether dianhydride; And S2, forming a film by using the polyamic acid solution to obtain a polyimide film.
  2. 2. The method according to claim 1, wherein in the step S1, the molar ratio of the 1, 12-diaminododecane to the 1, 3-bis (3-aminophenoxy) benzene in the mixed diamine monomer is (1 to 9): 1 to 9.
  3. 3. The method according to claim 1, wherein in the step S1, the molar ratio of the diamine monomer in the mixed diamine monomer to the dianhydride monomer is (0.98 to 1.02): 1.
  4. 4. The method for preparing a transparent shape memory polyimide film according to claim 1, wherein in the step S1, the time of the first stirring reaction is 23 to 25 hours.
  5. 5. The method for preparing a transparent shape memory polyimide film according to claim 1, wherein in the step S1, the first high boiling polar aprotic solvent includes at least one of N, N-dimethylformamide and N, N-dimethylacetamide.
  6. 6. The method according to claim 1, wherein in the step S2, the forming of the film using the polyamic acid solution comprises: adding acetic anhydride and pyridine into the polyamic acid solution, and carrying out a second stirring reaction to obtain a polyimide mixed solution; adding the polyimide mixed solution into ethanol to separate out, and collecting precipitate to obtain polyimide fibers; Dissolving the polyimide fiber in a second high-boiling-point polar aprotic solvent to obtain a polyimide solution; and coating the polyimide solution on a substrate, and drying to obtain the polyimide film.
  7. 7. The method of producing a transparent shape memory polyimide film according to claim 6, wherein the molar ratio of the acetic anhydride, the pyridine to the dianhydride monomer is (4 to 10): 1.
  8. 8. The method of producing a transparent shape-memory polyimide film according to claim 6, wherein the mass of the polyimide mixed solution is m g, the volume of the ethanol is v ml, and the ratio of m to v is 1 (9 to 11).
  9. 9. The method according to claim 1, wherein in the step S2, the forming of the film using the polyamic acid solution comprises: And coating the polyamic acid solution on a substrate, heating to 60-90 ℃, preserving heat for 1-3h, then heating to 100-150 ℃, preserving heat for 1-3h, then heating to 160-180 ℃, preserving heat for 1-3h, and finally heating to 190-210 ℃ and preserving heat for 1-3h to obtain the polyimide film.
  10. 10. A transparent shape memory polyimide film produced by the method of producing a transparent shape memory polyimide film according to any one of claims 1 to 9.

Description

Transparent shape memory polyimide film and preparation method thereof Technical Field The invention relates to the technical field of optical films, in particular to a transparent shape memory polyimide film and a preparation method thereof. Background Shape Memory Polymers (SMPs) exhibit broad application prospects in the fields of aerospace, biomedical and flexible electronics due to their programmable nature and ability to return from a temporary shape to a permanent shape under a variety of external stimuli such as heat, light, electricity, pH, etc. Among them, the Shape Memory Polyimide (SMPIs) has excellent heat stability, mechanical properties and radiation resistance inherent to polyimide, and has become a research hot spot for high temperature shape memory materials. In recent years, with the rapid development of flexible photovoltaic devices such as flexible perovskite solar cells, flexible displays and spatially self-expanding structures, there has been an urgent need for polymer materials having both optical transparency and shape memory functions. At present, the reported research of transparent shape memory polyimide mainly focuses on Gao Wenchu hair style materials, the glass transition temperature (Tg) of the hair style materials is generally above 150 ℃, and in practical application, a heating device is required to provide a high-temperature environment to realize the shape memory function, so that the hair style materials have high energy consumption and are difficult to be suitable for photoelectric devices sensitive to heat. On the other hand, although the conventional low-temperature shape memory polymers are easy to deform, most of the low-temperature shape memory polymers are opaque materials, have poor light transmittance and are difficult to apply to optical devices. Therefore, how to obtain a polyimide film with better transparency, better shape memory performance and lower glass transition temperature is a current problem to be solved. Disclosure of Invention The invention solves the problem of how to obtain the polyimide film with better transparency, better shape memory performance and lower glass transition temperature. In order to solve the above problems, the present invention provides a method for preparing a transparent shape memory polyimide film, comprising: step S1, uniformly mixing a mixed diamine monomer, a dianhydride monomer and a first high-boiling-point polar aprotic solvent in a protective gas atmosphere, and performing a first stirring reaction to obtain a polyamic acid solution, wherein the mixed diamine monomer comprises 1, 12-diaminododecane and 1, 3-bis (3-aminophenoxy) benzene, and the dianhydride monomer comprises bisphenol A type diether dianhydride; And S2, forming a film by using the polyamic acid solution to obtain a polyimide film. Optionally, in the step S1, the molar ratio of the 1, 12-diaminododecane to the 1, 3-bis (3-aminophenoxy) benzene in the mixed diamine monomer is (1 to 9): 1 to 9. Optionally, in step S1, the molar ratio of diamine monomer in the mixed diamine monomer to dianhydride monomer is (0.98 to 1.02): 1. Optionally, in the step S1, the time of the first stirring reaction is 23h to 25h. Optionally, in the step S1, the first high boiling polar aprotic solvent includes at least one of N, N-dimethylformamide and N, N-dimethylacetamide. Optionally, in the step S2, the film forming using the polyamic acid solution includes: adding acetic anhydride and pyridine into the polyamic acid solution, and carrying out a second stirring reaction to obtain a polyimide mixed solution; adding the polyimide mixed solution into ethanol to separate out, and collecting precipitate to obtain polyimide fibers; Dissolving the polyimide fiber in a second high-boiling-point polar aprotic solvent to obtain a polyimide solution; and coating the polyimide solution on a substrate, and drying to obtain the polyimide film. Alternatively, the molar ratio of the acetic anhydride, the pyridine, and the dianhydride monomer is (4 to 10): 1. Optionally, the mass of the polyimide mixed solution is m g, the volume of the ethanol is v milliliters, and the ratio of m to v is 1 (9 to 11). Optionally, in the step S2, the film forming using the polyamic acid solution includes: And coating the polyamic acid solution on a substrate, heating to 60-90 ℃, preserving heat for 1-3h, then heating to 100-150 ℃, preserving heat for 1-3h, then heating to 160-180 ℃, preserving heat for 1-3h, and finally heating to 190-210 ℃ and preserving heat for 1-3h to obtain the polyimide film. The invention also provides a transparent shape memory polyimide film, which is prepared by the preparation method of the transparent shape memory polyimide film. Compared with the related art, the polyimide film is prepared by reacting 1, 12-diaminododecane and 1, 3-bis (3-aminophenoxy) benzene serving as diamine monomers with bisphenol A type diether dianhydride, wherein the 1, 12-diaminododecane serving as a r