Polythioether acid imide and preparation thereof

A technology of polythioetherimide and phthalimide, which is applied in the field of preparing new polythioetherimide, can solve the problems of cumbersome preparation process and high polymer cost, and achieve reasonable and practical process and low cost , the effect of low melt viscosity

Inactive Publication Date: 2009-06-24
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since the above-mentioned reports all need to prepare thioether dianhydride first, t

Method used

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  • Polythioether acid imide and preparation thereof
  • Polythioether acid imide and preparation thereof
  • Polythioether acid imide and preparation thereof

Examples

Experimental program
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Embodiment 1

[0032]Add 182.56 grams (1.0mol) of 4-chlorophthalic anhydride and 1000 milliliters of glacial acetic acid into a dry and clean 2L three-necked flask, stir to dissolve and add 113.16 grams (0.5mol) of 3,3'-dimethyl-4,4'- Diaminodiphenylmethane (DMMDA), heated to 140°C for 24 hours, then cooled to room temperature, poured it into 10 liters of water, filtered to obtain a white solid, washed the filter cake three times with distilled water, and dried under vacuum at 120°C to obtain double Chlorine monomer crude product 249.9 grams, yield 90%. The crude product was recrystallized from dimethyl sulfoxide and used in the next polymerization reaction. Under an argon atmosphere, add 27.77 grams (0.05mol) of the above-mentioned dichloro monomer, 3.90 grams (0.05mol) of anhydrous sodium sulfide, 2.000 grams (0.05mol) of sodium hydroxide, and 300 milliliters of N , N'-dimethylacetamide (DMAc), heated to 120 ° C for 24 hours, cooled to room temperature, slowly poured the reaction solution...

Embodiment 2

[0034] Add 182.56 grams (1.0mol) of a mixture of 3-chlorophthalic anhydride and 4-chlorophthalic anhydride with a mass ratio of 5:1, 1000 milliliters of glacial acetic acid, and stir to dissolve and add 113.16 grams (0.5mol ) DMMDA, heated to 130 ° C for 24 hours, then cooled to room temperature and poured it into 10 liters of water, filtered to obtain a white solid, the filter cake was washed three times with distilled water, and vacuum-dried at 120 ° C to obtain 236 grams of dichloromonomer crude product , yield 85%. The crude product was recrystallized from a mixed solvent of DMAc and toluene (volume ratio 2:1) and used for the next polymerization reaction. Under a nitrogen atmosphere, add 27.77 grams (0.05mol) of the above-mentioned dichloromonomers, 3.90 grams (0.05mol) of anhydrous sodium sulfide, 6.36 grams (0.06mol) of anhydrous sodium carbonate in a dry and clean 500 milliliter three-necked flask, and 250 milliliters DMAc, heated up to 130°C for 36 hours, cooled to r...

Embodiment 3

[0036] Add 91.28 grams (0.5 mol) of a mixture of 3-chlorophthalic anhydride and 4-chlorophthalic anhydride in a dry and clean 1L three-necked flask with a mass ratio of 3:1, 500 ml of DMAc, stir to dissolve and add 49.56 grams (0.25mol) 4,4'-diaminodiphenylmethane (MDA), heated to 80°C for 2 hours, then heated to 130°C for 16 hours, then concentrated under reduced pressure to about 200 ml, poured into 3 liters of water, filtered to obtain White solid, the filter cake was washed three times with distilled water, and vacuum-dried at 120° C. to obtain 116 grams of crude dichloromonomer, with a yield of 88%. The crude product was vacuum melted and used for the next step of polymerization. Under a nitrogen atmosphere, add 26.37 grams (0.05mol) of the above-mentioned dichloromonomer, 2.30 grams (0.05mol) of anhydrous lithium sulfide, and 200 milliliters of N-methyl-2-pyrrolidone (NMP) in a dry and clean 500 milliliter three-necked flask. , heated up to 170°C for 8 hours, cooled to ...

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Abstract

The invention discloses a polythioether imide and a preparation method thereof. The method is characterized by comprising the following steps: chlorophthalic anhydride of a structural formula II is taken as a raw material of a reaction, and a half molar equivalent of disubstituted amine NH2RNH2 reacts at the temperature of about 100-200 DEG C to produce dichlorophthalimide; and a coupling reaction occurs between the dichlorophthalimide and alkali metal sulfide of the equal molar equivalent at the temperature of about 80-220 DEG C to produce polythioether imide resin of the structural formula I. The method has the advantages of saving raw materials and preparation cost, reducing reaction steps, having more rational and practical process, obtaining the resin with excellent all round properties such as good heat resistance, mechanical property and melt machining property, being capable of being widely applied to the related fields such as high-temperature resistant engineering plastic, film, adhesive, enameled wire, foam plastic, fiber, advanced composite material and the like.

Description

technical field [0001] The invention belongs to the technical field of polythioetherimides and related preparation methods, and in particular relates to a technical method for preparing novel polythioetherimides using chlorinated phthalic anhydride as a raw material and alkali metal sulfide as a coupling agent . Background technique [0002] Polythioetherimide is usually prepared by the reaction of thioether tetraacid dianhydride and aliphatic or aromatic diamine. Since the flexible unit of thioether bond is introduced into the rigid polyimide main chain, this kind of polymer has In addition to good thermomechanical properties, it also has the characteristics of good solubility, low melt viscosity and melt processability. It is a very promising thermoplastic heat-resistant polymer material. Therefore, the synthesis of thioether-type tetra-acid dianhydrides and corresponding polythioetherimides has attracted people's attention very early. For example, U.S. Patent Nos. 3,989...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08K3/30
Inventor 方省众马骥韩英胡本林严庆丁孟贤
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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