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Characterization method of interface combination condition of enhancement type hollow fiber membrane

A technology of interface bonding and fiber membrane, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of increased production cost, complicated equipment, and reduced membrane treatment effect, and achieve low equipment requirements and simple operation Effect

Inactive Publication Date: 2013-05-15
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Polyvinylidene fluoride (or polyacrylonitrile) hollow fiber membranes are widely used in the process of microfiltration and ultrafiltration due to their excellent performance. At present, the main method of preparation is the immersion precipitation method, and the membrane obtained by this wet method has a relatively high strength. Low, in the actual use of the membrane bioreactor (MBR), the membrane filaments are often damaged, which reduces the membrane treatment effect, shortens the service life, and increases the production cost. Hollow fiber membrane problems need to be solved
[0003] Chinese patent documents CN102068922A and CN102600733A both disclose a method for preparing a homogeneously reinforced polyvinylidene fluoride hollow fiber membrane, and Chinese patent document CN102580577A discloses a method for preparing a reinforced polyacrylonitrile hollow fiber membrane. Insufficient strength of hollow fiber membranes in MBR applications proposed better membrane preparation methods, but failed to describe and characterize the interfacial bonding of reinforced hollow fiber membranes in detail
[0004] D.Lian et al. (D.Lian, Y.Suga, G.Shou, and S.Kurihara.An UltrasonicTesting Method for Detecting Delamination of Sprayed Ceramic Coating.In:Proceedings of14th ITSC[C].Japan,1995.961~965) used ultrasonic A detector is used to test the bonding state between the coated ceramic layer and its substrate, and more reliable data can be obtained, but this method is complicated in equipment and can only detect materials with a separation diameter greater than 1mm
Within the scope of the applicant's search, there is currently no research report that directly characterizes the interfacial bonding of homogeneous reinforced membrane materials

Method used

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  • Characterization method of interface combination condition of enhancement type hollow fiber membrane
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  • Characterization method of interface combination condition of enhancement type hollow fiber membrane

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Preparation of homogeneously reinforced polyvinylidene fluoride hollow fiber membrane: mix 10% polyvinylidene fluoride with 10% polymethylpyrrolidone K30 by mass fraction, dissolve in 80% dimethyl ethyl ether In the amide solvent, stir in a water bath at 70°C for 3 hours to dissolve completely, and then defoam in a vacuum oven at 60°C to obtain a coating solution. Then, under the same spinning conditions, it is uniformly coated on the surface of the melt-spun polyvinylidene fluoride hollow fiber base membrane through a spinneret to prepare a homogeneously reinforced polyvinylidene fluoride hollow fiber membrane. The resulting hollow fiber membranes were soaked in ultrafiltered water at room temperature for 2 days before being tested.

[0032] Ultrasonic experiment: Put the homogeneously reinforced polyvinylidene fluoride hollow fiber membrane into an ultrasonic cleaner with an ultrasonic frequency of 40KHz. Take out multiple basement membranes as a group, to be tested....

Embodiment 2

[0035] Preparation of heterogeneously reinforced polyvinylidene fluoride hollow fiber membrane: mix 10% polyacrylonitrile with 10% polymethylpyrrolidone K30 by mass fraction, dissolve in 80% dimethylacetamide After stirring in a water bath at 70° C. for 3 hours to completely dissolve in the solvent, degassing in a vacuum oven at 60° C. to obtain a coating solution. Then, under the same spinning conditions, it is uniformly coated on the surface of the melt-spun polyvinylidene fluoride hollow fiber base membrane through a spinneret to prepare a heterogeneously reinforced polyvinylidene fluoride hollow fiber membrane. The resulting hollow fiber membranes were soaked in ultrafiltered water at room temperature for 2 days before being tested.

[0036] Ultrasonic experiment: Put the heterogeneously reinforced polyvinylidene fluoride hollow fiber membrane into the ultrasonic cleaner, the ultrasonic frequency is 40KHz, after the ultrasonic wave starts, it is respectively at 0min, 10min...

Embodiment 3

[0039]Preparation of homogeneously reinforced polyacrylonitrile fiber membrane: mix polyacrylonitrile with a mass fraction of 10% and polymethylpyrrolidone K30 with a mass fraction of 7%, and dissolve it in a solvent with a mass fraction of 83% dimethyl sulfoxide , stirred in a water bath at 70° C. for 3 hours to dissolve completely, and degassed in a vacuum oven at 45° C. to obtain a coating solution. Then, under the same spinning conditions, it is uniformly coated on the surface of the polyacrylonitrile fiber hollow braided tube through a spinneret to prepare a homogeneously reinforced polyacrylonitrile hollow fiber membrane. The resulting hollow fiber membranes were soaked in ultrafiltered water at room temperature for 2 days before being tested.

[0040] Ultrasonic experiment: put the homogeneously reinforced polyacrylonitrile hollow fiber membrane into the ultrasonic cleaner, the ultrasonic frequency is 40KHz, after the ultrasonic starts, respectively, at 0min, 5min, 10mi...

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Abstract

The invention discloses a characterization method of the interface combination condition of an enhancement type hollow fiber membrane. The characterization method comprises the following steps of: (1) enhancement type membrane sample preparation: (1) preparing a polyvinylidene fluoride-based enhancement type hollow fiber membrane sample: firstly preparing a polyvinylidene fluoride-based coating solution and a polyacrylonitrile-based coating solution, and then respectively uniformly coating the polyvinylidene fluoride-based coating solution and the polyacrylonitrile-based coating solution on the surface of a melt-spun polyvinylidene fluoride hollow fiber-based membrane through spinnerets to prepare a homogeneous enhancement type polyvinylidene fluoride hollow fiber membrane sample and a heterogenous enhancement type polyvinylidene fluoride hollow fiber membrane sample; and (2) preparing a polyacrylonitrile-based enhancement type membrane sample by the same method adopted in the step (1); (2) ultrasonic experiment: respectively placing the membrane samples prepared in the step (1) into an ultrasonic cleaner under the same condition for the ultrasonic experiment; and (3) flux test: carrying out pure water flux test on the membrane samples subjected to the ultrasonic experiment in the step (2), and indirectly characterizing the interface combination condition of the enhancement type hollow fiber membrane through obtained pure water flux change data.

Description

technical field [0001] The invention relates to a membrane quality detection technology, in particular to a method for characterizing the interfacial bonding state of a reinforced hollow fiber membrane. Background technique [0002] Polyvinylidene fluoride (or polyacrylonitrile) hollow fiber membranes are widely used in the process of microfiltration and ultrafiltration due to their excellent performance. At present, the main method of preparation is the immersion precipitation method, and the membrane obtained by this wet method has a relatively high strength. Low, in the actual use of the membrane bioreactor (MBR), the membrane filaments are often damaged, which reduces the membrane treatment effect, shortens the service life, and increases the production cost. Hollow fiber membranes are an urgent problem to be solved. [0003] Chinese patent documents CN102068922A and CN102600733A both disclose a method for preparing a homogeneously reinforced polyvinylidene fluoride hol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D65/10
Inventor 肖长发白倩倩张旭良胡晓宇环国兰
Owner TIANJIN POLYTECHNIC UNIV