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Method for preparing hollow fiber composite membrane

A technology of fiber composite and preparation process, applied in membrane technology, semi-permeable membrane separation, chemical instruments and methods, etc., to achieve the effect of simple process, superior separation and mechanical properties, and low manufacturing cost

Active Publication Date: 2011-11-02
蒋兰英
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, if the polymer has poor contact with the molecular sieve, it will be a difficult job to make it reproducible during the fiber coating process

Method used

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  • Method for preparing hollow fiber composite membrane
  • Method for preparing hollow fiber composite membrane
  • Method for preparing hollow fiber composite membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1、2、3、4

[0061] In all cases, the selection layer solution containing molecular sieve and polymer, the support layer solution and the core solution were the same and were prepared according to the following Table 1 recipe:

[0062] Table 1. Double-layer hollow fiber coating and core fluid composition

[0063]

[0064] The casting solution prepared according to the formula in Table 1 was extruded through a three-hole spinneret channel, and the hollow liquid flow thus formed was immediately condensed in water or passed through a certain air gap before being solidified in water. The precipitated solidified fibers are rolled up and collected by a cylinder. The different hollow fiber membranes prepared using the conditions shown in Table 2 are indicated by capital letters in brackets.

[0065] Table 2. Spinning conditions of double-layer hollow fibers.

[0066]

[0067] Afterwards, the fibers were soaked in clean tap water for at least three days to remove residual solvent, followed...

example 1、2、3

[0074] The air-dried hollow fiber membrane was heat-treated at 200°C (185°C higher than the glass transition temperature of polysulfone) and vacuum for two hours, and other conditions (fiber preparation and testing) were completely the same as those in Comparative Examples 1 to 4. unanimous. Thereafter, the first coating solution, i.e. 0.2wt% diethyltoluenediamine isooctane solution, the second coating solution, i.e. 0.2wt.% trimesoyl chloride isooctane solution, and the aforementioned The obtained 2wt.% silicone rubber solution was used to sequentially coat the outer layer of the hollow fiber membrane, and the coating time was 30 minutes. The above operations were carried out under the condition of vacuuming the inside of the membrane. After solvent removal, the fibers were further annealed at 100°C for two hours and stabilized in an oven for 2 days before testing. The thickness of the outer layer of the hollow fiber composite membrane thus produced is between 1 and 15 micr...

Embodiment 5、6

[0080] After solvent exchange between methanol and n-hexane, the air-dried hollow fiber membrane was immersed in 2.5% (g / cm3) p-xylylenediamine methanol solution for 1 hour. After being taken out and air-dried, the fiber membrane was annealed at 200° C. in vacuum for 2 hours. The fibers thus produced were coated in the same manner as in Examples 1-4. The test results of the obtained film are shown in Table 5:

[0081] Table 5. Permeability and selectivity of the hollow fiber membranes of Examples 5 to 6

[0082]

[0083] *x in the table represents the hollow fiber membrane cross-linked with p-xylylenediamine.

[0084] These fibers had very low permeability compared to those fibers in Table 4 that were not crosslinked with p-xylylenediamine. However, the separation selectivity of oxygen and nitrogen of fiber A is greatly improved, which deserves attention.

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Abstract

The invention relates to an asymmetric membrane, and in particular relates to a method for preparing a hollow fiber composite membrane. The method comprises the following steps: using an annular channel of a three-channel spinning nozzle at an outer layer to transmit a casting solution of mixed organic and inorganic materials at an outer layer; using an annular channel of the three-channel spinning nozzle at an intermediate layer to transmit of a casting solution of high polymers at a support layer; using a pipe in the middle of the three-channel spinning nozzle to transmit a core solution; immersing a hollow fiber membrane in a nascent state in a non-solvent coagulation bath; carrying out non-solvent phase change and curing on the casting solutions to form a membrane finally; and removing normal hexane and methyl alcohol hollow fiber membranes and carrying out crosslinking by using a chemical cross-linking agent, drying in air and carrying out high-temperature annealing and coating silicon rubbers to seal gaps. Compared with an existing method for preparing mixed organic and inorganic ultrathin membranes, the method in the invention has the advantages that: the method is simpler,thus being low in preparing cost; the materials are selected more flexibly, thus taking full advantage of characteristics of the different materials; and compared with the same type of membranes, theseparating property and the mechanical property are more superior.

Description

technical field [0001] The invention relates to an asymmetric membrane, especially a preparation process of a hollow fiber composite asymmetric membrane. Background technique [0002] In the field of gas separation, the importance of membrane separation is becoming more and more significant. Over the past few decades, polymer membranes have been the focus of attention in both academia and industry. This is due to the advantages of high polymer materials such as easy fabrication and easy processing. However, there is a challenge to further improve the separation effect of polymer membranes: there is a trade-off tendency between the permeate flux and separation factor of the membrane. This is mainly caused by the softness and thermal movement of the polymer chains. One of the ways to solve this problem in recent years is organic-inorganic blend matrix materials. [0003] The organic-inorganic blend composite membrane is to add uniformly dispersed inorganic particles into t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D69/08B01D67/00
Inventor 蒋兰英
Owner 蒋兰英
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