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Polyamic acid and preparation method thereof, and polyimide and polyimide fiber of polyamic acid

A technology of polyamic acid and polyimide, which is applied in the field of polyimide, can solve the problems of poor fiber performance uniformity and stability, random molecular chain structure sequence, and improve mechanical strength, so as to enhance the force between molecular chains , good mechanical properties, the effect of increasing density

Pending Publication Date: 2022-01-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention mainly solves one of the problems in the prior art. In the prior art, high-strength and high-model polyimide fibers generally use random copolymerization, which leads to random molecular chain structure sequences, lack of predictability, and poor fiber performance uniformity and stability, which is not conducive to Improvement of mechanical strength and further processing issues

Method used

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  • Polyamic acid and preparation method thereof, and polyimide and polyimide fiber of polyamic acid
  • Polyamic acid and preparation method thereof, and polyimide and polyimide fiber of polyamic acid
  • Polyamic acid and preparation method thereof, and polyimide and polyimide fiber of polyamic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0111] [Example 1] (the molar percentage of BPDA / BIA block segment in the total segment is 70%)

[0112] 1. Stock solution preparation: (1) Dissolve 5.48Kg (24.44mol) 2-(4-aminophenyl)-5-aminobenzimidazole (BIA) in 85Kg N,N-dimethylacetamide (DMAc) , at 25°C N 2 Stir under protection, after completely dissolving, add 6.47Kg (22.00mol) 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA), continue stirring for 1h after the addition, and obtain polyamic acid (PAA) polymer solution 1;

[0113] (2) The same polymerization condition, 0.75Kg (6.97mol) p-phenylenediamine (p-PDA) is dissolved in N,N-dimethylacetamide, 1.37Kg (6.27mol) pyromellitic dianhydride ( PMDA) was added in the diamine solution, fully stirred for 1.5h to obtain prepolymer solution 2;

[0114] (3) fully mix prepolymer solution 1 and prepolymer solution 2 for 1.5h to obtain prepolymer solution 3;

[0115] (4) Add 0.92Kg (3.14mol) 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA) into the prepolymer solution...

Embodiment 2

[0122] [Example 2] (BPDA / BIA segment accounted for 20% molar percentage of the total segment)

[0123] 1. Stock solution preparation: (1) Dissolve 1.99Kg (8.89mol) 2-(4-aminophenyl)-5-aminobenzimidazole (BIA) in 85Kg N,N-dimethylacetamide (DMAc) , at 25°C N 2 Stir under protection, after completely dissolving, add 2.35Kg (8.00mol) 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA), continue stirring for 1h after the addition, and obtain polyamic acid (PAA) polymer solution 1;

[0124] (2) Under the same polymerization conditions, 3.36Kg (31.12mol) p-phenylenediamine (p-PDA) was dissolved in N,N-dimethylacetamide, 6.11Kg (28.01mol) pyromellitic dianhydride ( PMDA) was added in the diamine solution, fully stirred for 1h to obtain prepolymer solution 2;

[0125] (3) fully mixing prepolymer solution 1 and prepolymer solution 2 for 1 h to obtain prepolymer solution 3;

[0126] (4) 1.18Kg (4.00mol) 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA) was added to the prepolyme...

Embodiment 3

[0128] [Example 3] (the molar percentage of BPDA / BIA block segment accounting for the total segment is 50%)

[0129] 1. Stock solution preparation: (1) Dissolve 3.98Kg (17.74mol) 2-(4-aminophenyl)-5-aminobenzimidazole (BIA) in 85Kg N,N-dimethylacetamide (DMAc) , at 25°C N 2 Stir under protection, after completely dissolving, add 4.70Kg (15.97mol) 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA), continue stirring for 1h after the addition, and obtain polyamic acid (PAA) polymer solution 1;

[0130] (2) Under the same polymerization conditions, 2.84Kg (14.19mol) 4,4'-diaminodiphenyl ether (ODA) was dissolved in N,N-dimethylacetamide, and 2.78Kg (12.78mol) pyromellitic Acid dianhydride (PMDA) was added to the diamine solution, and fully stirred for 1 hour to obtain prepolymer solution 2;

[0131] (3) fully mixing prepolymer solution 1 and prepolymer solution 2 for 1 h to obtain prepolymer solution 3;

[0132] (4) 0.69Kg (3.19mol) pyromellitic dianhydride (PMDA) was added...

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Abstract

The invention discloses polyamic acid and a preparation method thereof and a polyimide fiber of the polyamic acid. The polyamic acid comprises chain segments a and chain segments b, wherein the chain segments a have at least one of structures as shown in a formula 1 and a formula 2; the chain segments b have a structure as shown in a formula 3; links between the chain segments a, between the chain segments b and / or between the chain segments a and the chain segments b comprise a structure as shown in a formula 4; and the chain segments a and the chain segments b are different. The polyimide fiber disclosed by the invention is good in uniformity, stability and mechanical property and beneficial to subsequent processing. The breaking strength of the polyimide fiber is greater than 3.0 GPa, and CV is less than or equal to 5%; and the modulus of the polyimide fiber is greater than 100 GPa, and CV is less than or equal to 5%.

Description

technical field [0001] The invention relates to the field of polyimide, in particular to a polyamic acid, a preparation method thereof, polyimide and polyimide fiber thereof. Background technique [0002] Polyimide (PI) is a kind of polymer with imide ring as the characteristic structure. As a polymer material with outstanding comprehensive performance, it has a wide range of uses. and other important fields have been applied. PI has a wide range of synthesis methods and many processing and molding methods, and has become a development hotspot in the engineering plastics industry in the world today. [0003] In the current polyimide (PI) preparation process, the two-step synthesis method is the most widely used synthesis method. That is, firstly, diamine and dianhydride monomers are successively added into a suitable stirring solvent, and at this time, a polyamic acid (PAA) solution is prepared by low-temperature condensation polymerization. When preparing PI fibers, the ...

Claims

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Application Information

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IPC IPC(8): C08G73/10D01F6/78
CPCC08G73/1085C08G73/1067C08G73/1028C08G73/1042D01F6/78
Inventor 陈雪崔晶孙旭阳林程
Owner CHINA PETROLEUM & CHEM CORP
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