Preparation method for poly(p-phenylene terephthamide) membrane

The technology of poly-p-phenylene terephthalamide and terephthaloyl chloride is applied in the field of preparation of poly-p-phenylene terephthalamide film, which can solve the problems of difficult process control and high production cost, and achieves the Improve film-forming performance and pore-forming performance, process safety, and optimize the effect of production processes

Active Publication Date: 2015-03-11
TSINGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solution phase inversion method can effectively control the structure of the film, but the production cost is high and the process control is difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0011] The preparation method of the poly-p-phenylene terephthalamide film that the present invention proposes comprises the following steps:

[0012] (1) Polymerization: Add solvent N to methylpyrrolidone (hereinafter referred to as NMP) into the reactor, add polymerization aids and surfactants while stirring under nitrogen protection and a rotating speed of 50 to 300 rpm, and heat the reactor to 70 ~100°C and constant temperature until the auxiliary agent and surfactant are dissolved, then the reactor is cooled to 0-30°C, and the first polymerized monomer p-phenylenediamine (hereinafter referred to as PPD) is added to make the molar concentration of p-phenylenediamine After the p-phenylenediamine is completely dissolved, the temperature of the reactor is lowered to -15-10°C, and then the second polymerization monomer terephthaloyl chloride (hereinafter referred to as TPC) is added for polymerization, so that the p-phenylenediamine The molar concentration of phthaloyl chlorid...

Embodiment 1

[0020] 1) Add 100mL NMP to a 300ml reactor, add 10g of polymerization aid CaCl under nitrogen protection and stirring 2 and 5g of polyethylene glycol (PEG) with a molecular weight of 2100, heated to 100°C to dissolve the auxiliary agent and surfactant. To be CaCl 2 After the PEG and PEG are completely dissolved, the system is lowered to 15°C with an ice-water bath, and then 4.326g of p-phenylenediamine (PPD) is added to dissolve. After the PPD is completely dissolved, 8.178g of terephthaloyl chloride (TPC) is added and stirred at a high speed (2000r / min ) for polymerization, keep an ice-water bath during the polymerization process, and keep the system temperature not exceeding 70°C;

[0021] 2) The above polycondensation reaction proceeds until the system forms a jelly body and the Weissenberg effect occurs, stop stirring, remove the ice-water bath, take out 5 g of the jelly body and add 200 ml of NMP, stir the swollen jelly body for 5 minutes quickly with a tissue grinder, a...

Embodiment 2

[0024] 1) Add 100mL NMP to a 300ml reactor, add 8g of polymerization aid LiCl and 5g of polyethylene glycol (PEG) with a molecular weight of 2100 and an ethyl end group under nitrogen protection and stirring, and heat to 100°C to make the aid and The surfactant dissolves. After LiCl and PEG are completely dissolved, use an ice-water bath to lower the system to 10°C, then add 4.326g of p-phenylenediamine (PPD) to dissolve, and then add 8.160g of terephthaloyl chloride (TPC) after PPD is completely dissolved and stir at a high speed (2000r / min) to carry out polymerization, keep an ice-water bath during the polymerization process, and keep the system temperature not exceeding 60°C;

[0025]2) The above polycondensation reaction is carried out until the system forms a jelly body and the Weissenberg effect occurs, stop stirring, remove the ice-water bath, take out 5g of the jelly body and add 300ml of NMP, stir the swollen jelly body for 5 minutes with a tissue pulverizer, break u...

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PUM

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Abstract

The invention relates to a preparation method for a poly(p-phenylene terephthamide) (PPTA) membrane, and belongs to the technical field of membrane materials and polymer polymerication. The preparation method comprises: adding a certain amount of a surfactant in a PPTA low-temperature solution polymerization process, adding a large amount of a solvent N-methylpyrolidone (NMP) into the polymerization system after polymerization is performed to a certain degree, so as to disperse the polymerization system, then adding a large amount of a dispersing agent to washing out the surfactant, and then performing reduced-pressure filtering on the PPTA dispersion solution, so as to obtain the membrane. The preparation method starts from a PPTA monomer, and the high-performance PPTA membrane with small shrinkage, high strength and isotropy is prepared through steps of polymerization, swelling, dispersing, filtering and drying. The employed surfactant is soluble polyoxyethylene ether high molecules with different molecular weight and different end groups, and the dispersing agent employs water, alcohols and other polar solvents. The preparation method has the characteristics of being simple and practicable in membrane preparation technology, safe in process, efficient, controllable and the like, and has good industrial application prospect.

Description

technical field [0001] The invention relates to a method for preparing a poly-p-phenylene terephthalamide film, belonging to the technical field of membrane materials and polymer polymerization. technical background [0002] Poly(p-phenylene terephthalamide) (hereinafter referred to as PPTA) is a liquid crystal polymer. The PPTA molecular chain contains a large number of conjugated benzene rings and amide structures, which are very rigid and form a large number of hydrogen bonds between the molecular chains, so it has many advantages such as low density, high strength, high modulus and heat resistance. The fiber prepared therefrom is a high-performance fiber (para-aramid, aramid 1414 or aramid II), which is widely used in the fields of aerospace, military equipment, building materials and sports equipment. [0003] PPTA film is as widely used as fiber. It plays an irreplaceable role in many fields such as electric power, high-speed rail, aircraft, and sealing. At present,...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08L77/10C08G69/32C08G69/28
Inventor 庹新林闫鸿琛李京龙郭澄龙许甲崔庆海
Owner TSINGHUA UNIV
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