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A kind of preparation method of soluble and meltable copolymerization polyimide molding compound

A polyimide and polyamic acid technology, which is applied in the field of preparation of soluble and fusible copolymerized polyimide, can solve the problems of reducing polymer solubility and thermoplasticity, affecting processing performance, etc., so as to improve thermal performance, The processing performance is equivalent, and the effect of easy filtration and separation

Active Publication Date: 2016-06-29
SHANGHAI PLASTICS RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, increasing the composition of the rigid segment in the polymer segment can effectively increase the glass transition temperature Tg of the polymer, but the increase of the rigid component will reduce the solubility and thermoplasticity of the polymer, thereby affecting the processing performance

Method used

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  • A kind of preparation method of soluble and meltable copolymerization polyimide molding compound
  • A kind of preparation method of soluble and meltable copolymerization polyimide molding compound
  • A kind of preparation method of soluble and meltable copolymerization polyimide molding compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Put 160g (0.8mol) of 4,4'-diaminodiphenyl ether, 21.6g (0.2mol) of p-phenylenediamine and 2200ml of diphenylenediamine into a 5000ml four-neck round bottom flask equipped with a mechanical stirrer, a thermometer, and a nitrogen inlet and outlet. Methyl acetamide, stir to dissolve completely, then add 310g (1mol) 2,3,3′,4′-diphenyl ether tetracarboxylic dianhydride, react at room temperature for 4 hours to obtain a polyamic acid solution, add 1050g acetic anhydride , triethylamine 260g and xylene 210g, continue to react for 1.0 to complete the imidization reaction, filter the precipitated polyimide powder, then wash with 1000ml acetone three times, filter, and bake at 50-80°C for 1-2 hours , and then heat-treated at 220°C to 280°C for 2 to 5 hours to obtain a copolymerized polyimide with a yield of 92% and an inherent viscosity of 75ml / g. The polyimide molded a plastic sample at 350°C / 30MPa, and the performance indicators of the plastic sample are shown in Table-1 below:...

Embodiment 2

[0048] Put 100g (0.5mol) of 4,4'-diaminodiphenyl ether, 54g (0.5mol) of p-phenylenediamine and 2200ml of dimethyl Acetamide, stir to dissolve completely, then add 310g (1mol) 2,3,3′,4′-diphenyl ether tetracarboxylic dianhydride, and react at room temperature for 4 hours to obtain a polyamic acid solution, and then proceed with the implementation Example 1 is the same. The yield of the molding powder was 88.3%, the logarithmic viscosity was 61.5ml / g, the glass transition temperature (Tg) was 303°C, and the weight loss temperatures of 5% and 10% were 551°C and 577°C, respectively (see Table 2).

[0049] Table-2: The mechanical properties of the copolyimide obtained in embodiment 2

[0050]

[0051] Bending strength, MPa

Embodiment 3

[0053] Put 130g (0.65mol) of 4,4′-diaminodiphenyl ether, 37.8g (0.35mol) of p-phenylenediamine and 2200ml of diphenylenediamine into a 5000ml four-neck round bottom flask equipped with a mechanical stirrer, a thermometer, and a nitrogen inlet and outlet. Methyl acetamide, stir and dissolve completely, then add 310g (1mol) 2,3,3′,4′-diphenyl ether tetracarboxylic dianhydride, react at room temperature for 4 hours to obtain a polyamic acid solution, and then proceed with Example 1 is the same. The yield of the molding powder was 88.6%, the logarithmic viscosity was 67.5ml / g, the glass transition temperature Tg was 294°C, and the weight loss temperatures of 5% and 10% were 541°C and 581°C, respectively (see Table- 3).

[0054] Table-3: Mechanical properties of the copolyimide obtained in Example 3

[0055]

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Abstract

The invention discloses a method for preparing soluble meltable copolymerized polyimide molding plastic. The method comprises the following steps: preparing polyamide acid from 2,3,3',4'-diphenyl ether pyromellitic dianhydride(a-ODPA), 4,4'-diaminodiphenyl ether(4,4'-ODA) and 1,4-p-phenylenediamine(1,4-PDA) in a ternary polymerization manner together with a mixture of aromatic bianhydride and aromatic diamine through equal molar ratio reaction at room temperature, subsequently adding acetic anhydride, triethylamine and xylene to perform chemical imidization, subsequently filtering, washing in acetone, filtering, drying, screening through a sieve of 100 meshes so as to obtain a copolymerized polyimide powder material, and subsequently performing thermal treatment for 2-3 hours at 220-280 DEG C so as to completely imidize. The prepared copolymerized polyimide powder material has the logarithmic viscosity number of 40ml / g to 110ml / g, the 10wt% loss temperature is 577 DEG C, the retention rate of the tensile strength, the compression strength and the bending strength of a plastic component at 220 DEG C is not greater than 3-5% of that of a homopolymer without 1,4-PDA, and the thermal weight loss temperature and Tg are both increased by 11-12 DEG C.

Description

1. Technical field [0001] The present invention relates to a kind of preparation method of soluble and fusible copolymerization polyimide, relate to 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride and 4,4'-diamino dicarboxylic acid dianhydride more precisely The invention discloses a method for preparing copolymerized polyimide by reacting phenylene ether and p-phenylenediamine. 2. Background technology [0002] Polyimide has been highly valued by people for its excellent high temperature resistance, low temperature resistance, solvent resistance, radiation resistance, outstanding mechanical strength and dielectric properties, and has been widely used in aerospace, automotive industry, microelectronics, Flat panel display and many other high-tech fields. Developed by DuPont since the early 1960s Since the film, it has a history of nearly 50 years. This polyimide obtained by linear polymerization of pyromellitic dianhydride (PMDA) and diphenyl ether diamine (4,4'-ODA...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C08L79/08B29C43/58
Inventor 包来燕吕凯邱孜学贺飞峰
Owner SHANGHAI PLASTICS RES INST CO LTD
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