Preparation method of colorless transparent polyimide film with low yellowness and high mechanical property

A technology of transparent polyimide and polyimide resin, applied in the field of polymer materials, can solve the problems of poor stability, unsuitable for mass addition of cellulose, compatibility limitation, etc., so as to eliminate internal stress and improve optical transparency. Sex, the effect of eliminating yellowing

Active Publication Date: 2022-05-03
NINGBO CHANGYANG TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above-mentioned patents, the mechanical properties of the film are improved by introducing cellulose into the polyimide material, but in this solution, the cellulose is loaded in nano-alumina, and the cellulose is only dispersed in the polyimide by physical blending. In the imine substrate, due to the limitation of compatibility, the stability is poor, and it is easy to precipitate after aging in the later stage, and this method is not suitable for adding a large amount of cellulose
[0006] In addition, the traditional methods of reducing the yellowness of polyimide films are mainly accomplished by adding fluorine-containing monomers, introducing bulky substituents, main chain bending structures, asymmetric structures, and reducing conjugated double bond structures. It is mainly to reduce the intramolecular or intermolecular charge transfer, thereby reducing the formation of electron transfer complexes (CTCs) and improving the light transmittance and transparency of polyimide films, but these methods have no effect on the amino groups formed by diamine residues. Insufficient attention is paid to the yellowing caused by high temperature

Method used

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  • Preparation method of colorless transparent polyimide film with low yellowness and high mechanical property

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preparation example Construction

[0044] A preparation method of a colorless and transparent polyimide film with low yellowness and high mechanical properties, comprising the following steps:

[0045] (1) Dissolve alicyclic diamine in polar aprotic organic solvent A, add aminated nanocellulose (amino content is 1.3-1.8mmol / g, molecular weight is 5000-8000, diameter is 10-20nm, long 100-300nm), stirring continuously at 100-1500r / min for 5-20min, then adding alicyclic dianhydride in 2-10 times, stirring continuously for 5-24h at 0-10°C under nitrogen protection to obtain a polyamic acid solution. The molar ratio of the alicyclic diamine to the alicyclic dianhydride is 1.1-1:1-1.1, and the mass of the aminated nanocellulose is 1-10% of the alicyclic dianhydride. in:

[0046] Described cycloaliphatic diamine comprises 1,3-cyclohexanediamine, 1,4-cyclohexanediamine, 1,3-cyclobutanediamine, 4,4-diaminodicyclohexylmethane (PACM ) and one or more of 3,3-dimethyl-4,4-diaminodicyclohexylmethane (DMDC).

[0047] The c...

Embodiment 1

[0057] Add 11.4189g (0.1mol) of 1,4-cyclohexanediamine and 150g of N,N-dimethylacetamide (DMAC) into a 500mL three-necked flask equipped with a mechanical stirrer, a thermometer and a reflux condenser. Introduce nitrogen gas, and mechanically stir at 500 r / min for 20 min to obtain a clear solution. Then add 1.1209g of aminated nanocellulose (amino content is 1.3-1.8mmol / g, molecular weight is 5000-8000, diameter is 10-20nm, length is 100-300nm), continue to stir at 500r / min for 20min and divide into 5 times 22.4170 g (0.1 mol) of hydrogenated pyromellitic dianhydride (HPMDA) were added. Under the reaction condition of 5° C., stirring was continued at 500 r / min for 6 h to obtain a polyamic acid solution. Add 1.1209g carboxylated nanocellulose (carboxyl content is 1.2-3mmol / g, molecular weight is 5000-8000, diameter is 10-20nm, length is 100-300nm), 0.5g pyridine and 0.5g Acetic anhydride, continue stirring at 500 r / min for 6 h under nitrogen protection and reaction conditions...

Embodiment 2

[0060] The specific operations and conditions of Example 2 are the same as in Example 1, except that the used alicyclic diamine and alicyclic dianhydride are replaced by 1,3-cyclobutanediamine and 1,2,3,4-cyclobutanediamine respectively. Butane tetracarboxylic dianhydride (CBDA).

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Abstract

The invention relates to the field of high polymer materials, and discloses a preparation method of a colorless transparent polyimide film with low yellowness and high mechanical property. Aminated nanocellulose and carboxylated nanocellulose are introduced into a full-fat ring type polyimide film; the aminated nanocellulose and the carboxylated nanocellulose respectively serve as diamine monomers and end-capping reagents, can participate in the reaction of alicyclic diamine and alicyclic dianhydride and are doped into a polyimide polymer main chain in a covalent bond form, the stability is good, the mechanical property and the heat resistance of the polyimide film can be improved, and the polyimide film can be used as a polyimide film. The high-temperature yellowing effect caused by amino groups on diamine can also be inhibited. The finally prepared polyimide film still has relatively high mechanical and heat-resistant properties while the light transmittance is greater than 90%.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a preparation method of a colorless and transparent polyimide film with low yellowness and high mechanical properties. Background technique [0002] Polyimide is a kind of high molecular polymer containing imide units in the main chain. It has excellent heat resistance, mechanical properties, chemical stability and dielectric properties, so it is widely used in aerospace, semiconductor packaging, Solar cells and other fields. [0003] In recent years, the vigorous development of flexible display products, especially flexible mobile phones and flexible wearable devices, has put forward higher requirements for the bendability of materials. Traditional glass substrates have been difficult to meet the requirements, and polyimide films have excellent durability. Thermal and mechanical properties, which have attracted more and more attention, are regarded as one of the best materials ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L79/08C08G73/10
CPCC08J5/18C08G73/10C08J2379/08Y02E10/549
Inventor 张涛宋明雄熊斐杨帆张文浩
Owner NINGBO CHANGYANG TECH
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