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Preparation method of polythioetherimide

A technology of polythioetherimide and phthalimide, which is applied in the field of polymer resin preparation, can solve the requirements of polyetherimide resin with limited molecular weight, limited nucleophilic substitution reactivity, and difficulty in meeting the requirements of fiber grade, etc. problems, to achieve excellent mechanical properties and heat resistance, easy processing, good heat resistance and mechanical properties

Active Publication Date: 2014-01-08
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

All of the above are polyetherimides formed by self-condensation polymerization of A-B type monomers containing hydroxyl groups. Due to the limited reactivity of nucleophilic substitution of hydroxyl groups, the molecular weight of the obtained polyetherimide resins is limited, and it is difficult to meet the requirements of fiber grades. Even It is difficult to form a film, which limits its application in the field of film materials and fibers

Method used

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  • Preparation method of polythioetherimide
  • Preparation method of polythioetherimide
  • Preparation method of polythioetherimide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048]Add 19.3g (0.1mol) of 4-nitrophthalic anhydride, 19.3g (0.1mol) of 4-mercaptotrifluoromethylaniline, and 200mL of xylene into a dry and clean 500mL three-necked flask, and reflux at 150°C for 12 hour, cooled to room temperature, filtered, and the obtained filter cake was washed three times with toluene, and then placed in a vacuum oven at 80°C for 8 hours to obtain 33.4 g of light yellow A-B type phthalimide powder, with a yield of 93%. Characterize its structure by Fourier transform infrared spectrometer, the result is FT-IR (KBr): ν=1773(asym C=O stretching), 1712(sym C=O stretching), 1386(C-N stretching), 732(C =O bending). The reaction process is shown in the following formula:

[0049]

[0050] Add 8.1g (0.02mol) of compound III-1, 0.53g (0.022mol) of sodium hydride, and 30mL of dimethylacetamide into a dry and clean 100mL three-neck flask, and react at 160°C for 12 hours under the protection of nitrogen, and a polymer precipitates Precipitate, add 0.268g (0.00...

Embodiment 2

[0057] Add 16.6g (0.1mol) of 3-fluorophthalic anhydride, 24.3g (0.1mol) of 4-mercaptopropyleneaniline, 200mL of xylene into a dry and clean 500mL three-necked flask, and react under reflux at 150°C for 12 hours under nitrogen protection. Cool to room temperature, filter, and wash the obtained filter cake three times with toluene, and then place it in a vacuum oven at 80°C for 8 hours to obtain 36.4 g of pale yellow A-B type phthalimide powder, with a yield of 89%. Characterize its structure by Fourier transform infrared spectrometer, the result is FT-IR (KBr): ν=1772(asym C=O stretching), 1715(sym C=O stretching), 1385(C-N stretching), 730(C =O bending). The reaction process is shown in the following formula:

[0058]

[0059] Add 7.82g (0.02mol) of compound III-2, 2mL (0.022mol) of tri-n-butylamine, and 30mL of dimethylacetamide into a dry and clean 100mL three-necked flask, and react at 160°C for 12 hours under the protection of nitrogen. Precipitate, add 0.258g (0.001m...

Embodiment 3

[0066] Add 18.3g (0.1mol) 4-chlorophthalic anhydride, 26.5g (0.1mol) 4-mercaptosulfonylaniline, and 200mL toluene into a dry and clean 500mL three-necked flask, and reflux at 150°C for 12 hours under nitrogen protection, then cool to After filtering at room temperature, the obtained filter cake was washed three times with toluene, and then dried in a vacuum oven at 80°C for 8 hours to obtain 41.6 g of light yellow A-B type phthalimide powder, with a yield of 93%. Characterize its structure by Fourier transform infrared spectrometer, the result is FT-IR (KBr): ν=1775(asym C=O stretching), 1712(sym C=O stretching), 1383(C-N stretching), 729(C =O bending). The reaction process is shown in the following formula:

[0067]

[0068] Add 8.60g (0.02mol) of compound III-3, 3.04062g (0.022mol) of K 2 CO 3 , 30mL dimethyl sulfoxide, under the protection of nitrogen, reacted at 180°C for 12 hours, a polymer precipitated out, and added 0.258g (0.001mol ), continue to react for 2 hou...

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Abstract

The invention discloses a preparation method of polythioetherimide. The preparation method comprises the following steps: performing condensation polymerization on monosubstituted phthalic anhydride and aminothiophenol, serving as raw materials, to synthesize A-B type phthalimide monomer, dissolving the monomer in an organic solvent, mixing with an alkaline catalyst under the protection of nitrogen or inert gas and reacting at the temperature of 120-180 DEG C for 6-12 hours; adding a chain blocking agent, continuously reacting for 0.5-2 hours and then cooling; precipitating, filtering, washing and drying to obtain the polythioetherimide, wherein the monosubstituted phthalic anhydride has a structural formula I, and X can be fluorine, chlorine, bromine, iodine or nitro group and is at the 3-site or 4-site; the aminothiophenol has a structural formula II, and R is an aromatic group; the A-B type phthalimide monomer has a structural formula III. The invention provides a simple and feasible method for preparing the polythioetherimide; the method has a simple synthesis process; the prepared polythioetherimide has superior mechanical performance and heat resistance performance.

Description

technical field [0001] The invention relates to the field of preparation of polymer resins, in particular to a preparation method of polythioetherimide. Background technique [0002] Polyimide is a kind of high-performance resin with excellent comprehensive properties. It has good thermal stability, excellent mechanical properties, good dimensional stability, excellent chemical stability, high breakdown voltage, low dielectric constant, Excellent comprehensive properties such as high flame retardancy and low expansion coefficient are widely used in high-tech fields such as electronic appliances, aerospace, mechanical and chemical industries. [0003] The synthesis method of polyimide can generally be divided into two types: one is to use dianhydride and diamine as raw materials to form intermediate polyamic acid, and polyamic acid is dehydrated and cyclized to form polyimide. However, dianhydride storage When it is easy to hydrolyze into acid, diamine is easy to oxidize in ...

Claims

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Application Information

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IPC IPC(8): C08G75/04
Inventor 方省众刘江涛陈国飞
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI