Method for preparing polyimide hollow fiber

A polyimide, hollow technology, applied in the field of preparation of polyimide hollow fibers, can solve the problems of difficult removal, high toxicity, and many solvent residues

Inactive Publication Date: 2012-07-04
苏州乐华新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For a small number of soluble polyimides, one-step method can be used for fiber spinning, which is conducive to maintaining the supramolecular structure of polyimides, but usually uses phenolic solvents such as cresol and p-chlorophenol, which are not only toxic, but also There are many solvent residues in the fiber and it is difficult to remove completely

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Example 1: Dissolve polyimide in NMP (N-methyl-2-pyrrolidone) to prepare a polyimide spinning stock solution with a concentration of 7% by mass, and leave it for one day until the polyimide is completely dissolved After filtration and vacuum defoaming; porogen PEG (polyethylene glycol, M n =6000g / mol) was dissolved in methanol to make a core liquid with a mass percentage concentration of 12%, the flow rate of the core liquid was controlled to 0.2L / h, and the dry spinning distance was adjusted to 8cm, and the spinning after filtration and vacuum defoaming The crude polyimide hollow fiber is obtained by dry-jet wet spinning through a spinning machine, and the crude polyimide hollow fiber is placed in a coagulation bath with a temperature of 20 ° C and a volume ratio of alcohol and water made from methanol to 1 / 4. Cool in medium, wrap the cooled crude polyimide hollow fiber with filter paper, use distilled water as the extractant, boil and reflux for 24 hours to completely...

Embodiment 2

[0011] Example 2: Polyimide was dissolved in DMSO (dimethyl sulfoxide) to form a polyimide spinning stock solution with a concentration of 10% by mass, and it was placed for one day until the polyimide was completely dissolved, then filtered and dried. Vacuum defoaming; PEO (polyethylene oxide, M n =5000g / mol) dissolved in methanol to make a core liquid with a mass percentage concentration of 16%, control the flow rate of the core liquid to 0.5L / h, adjust the dry spinning distance to 6cm, filter and defoam the polyimide The spinning stock solution is dry-jet-wet spun by a spinning machine to obtain crude polyimide hollow fibers. Cool in a coagulation bath, wrap the cooled crude polyimide hollow fiber with filter paper, use distilled water as the extractant, boil and reflux for 24 hours to completely remove the residual porogen and solvent, take it out, and dry it in an oven To constant weight, the pure finished polyimide hollow fiber is obtained. It has been determined that ...

Embodiment 3

[0012] Example 3: Polyimide is dissolved in DMF (N, N-dimethylformamide) to form a polyimide spinning stock solution with a concentration of 12% by mass, and the polyimide is left for 1 day After complete dissolution, filter and vacuum defoam; PVP (polyvinylpyrrolidone, M n =6200g / mol) was dissolved in ethanol to make a core liquid with a mass percentage concentration of 24%, the flow rate of the core liquid was controlled to 0.8L / h, the distance of the dry spinning process was adjusted to 4cm, and the spinning dope after degassing was spun The crude polyimide hollow fiber is obtained by dry-jet wet spinning on a silk machine, and the obtained crude polyimide hollow fiber is cooled in a coagulation bath with a temperature of 30 ° C and an alcohol-water volume ratio of 4 / 1 made from ethanol. Wrap the cooled crude polyimide hollow fiber with filter paper, use distilled water as the extractant, and boil and reflux for 24 hours to completely remove the residual porogen and solvent...

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Abstract

The invention discloses a method for preparing a polyimide hollow fiber. The method comprises the following steps of: (1) dissolving polyimide in any solvent of dimethyl sulfoxide (DMSO) or dimethylformamide (DMF) or N-methyl-2-pyrrolidone (NMP) or tetrahydrofuran (THF) or acetone to prepare a 7 to 12 mass percent polyimide spinning stock solution, and defoaming and filtering after the polyimide is completely dissolved; (2) preparing a 12 to 24 mass percent core solution by taking any of polyoxyethylene (PEO) or polyethylene glycol (PEG) or polyvinylpyrrolidone (PVP) as a pore-forming agent and taking methanol or ethanol as a solvent; (3) adjusting flow of the core solution to 0.2 to 0.8L/h and distance of a dry spinning path to 4 to 8cm, and preparing a coarse polyimide hollow fiber from the stock solution obtained the step (1) through a spinning machine by a dry jet wet spinning method; (4) cooling the coarse polyimide hollow fiber; and (5) extracting the cooled coarse polyimide hollow fiber, drying to constant weight, and thus obtaining the finished polyimide hollow fiber.

Description

technical field [0001] The invention relates to a preparation method of a polyimide hollow fiber. Background technique [0002] Polyimide refers to a class of polymers containing imide rings in the main chain. It is a variety of industrialized polymer materials with excellent comprehensive properties. It has been widely used in aerospace, microelectronics, nano, liquid crystal, Separation membrane, laser and other fields. The gas separation membrane made of polyimide hollow fiber is 2 , CO 2 and O 2 Has high gas permeability and selectivity, especially for H 2 The high permeability can be used to prepare high-purity H 2 , Therefore, the polymer gas separation membrane made of this polyimide hollow fiber, that is, the polyimide separation membrane, has a huge potential application prospect in the aerospace field. [0003] The polymer membranes currently on the market are mainly used to remove CO from natural gas. 2 Compared with these two polymer membranes, the polyimi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/56B01D69/08B01D67/00
Inventor 刘河洲康红梅李华张菊陶文燕何庭清
Owner 苏州乐华新材料有限公司
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