Preparation method for microporous polyphenylene sulfide hollow fiber membrane

A technology of polyphenylene sulfide and fiber membrane, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of uneven pores and low flux, slow down the crystallization speed, and reduce the phase separation temperature , the effect of enhancing the strength

Active Publication Date: 2018-11-30
TIANJIN POLYTECHNIC UNIV
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  • Application Information

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Problems solved by technology

The literature "Wang Lihua. Research on Polyphenylene Sulfide Hollow Fiber Microfiltration Membrane [D]. Tianjin University of Technology, 2000" used a melt spinning machine for thermal stretching after melt spinning to prepare a PPS hollow fiber microfiltration membrane; studied The influence of spinning temperature, spinning speed and nitrogen flux on the formation of PPS hollow fiber membrane; but there are disadvantages such as uneven pores and low flux

Method used

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  • Preparation method for microporous polyphenylene sulfide hollow fiber membrane
  • Preparation method for microporous polyphenylene sulfide hollow fiber membrane
  • Preparation method for microporous polyphenylene sulfide hollow fiber membrane

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preparation example Construction

[0023] The invention provides a kind of preparation method (abbreviation method) of microporous polyphenylene sulfide hollow fiber membrane, it is characterized in that the method comprises the steps:

[0024] 1) The diluent is ground into powder at room temperature, and then the diluent accounting for 20-60% of the total mass, the porogen accounting for 0-2% of the total mass, the inorganic nanoparticles accounting for 0-2% of the total mass and The polyphenylene sulfide accounting for 40-80% of the total mass is uniformly mixed in a stirrer to obtain a homogeneous polyphenylene sulfide casting solution; the sum of the four mass is 100%;

[0025] The diluent is a benign diluent and an auxiliary diluent; the benign diluent is caprolactam (CPL), benzophenone (BP), diphenyl ether (DPE), benzoin (BZ) or diphenylsulfone (DPS) at least one of; the auxiliary diluent is dibutyl sebacate (DBS), dibutyl phthalate (DBP), dioctyl phthalate (DOP) or dioctyl isophthalate fat (DOTP);

[0...

Embodiment 1

[0038] (1) Batching (PPS: BP: BZ = 80%: 10%: 10%), the pulverizer is pulverized and mixed evenly, and the heating temperature of each segment of the screw section is set (240°C, 282°C, 294°C, 290°C, 290°C ℃, 292 ℃), spinneret temperature and metering pump temperature (264 ℃, 264 ℃), after the temperature is stable, adjust the main engine speed, feeding speed and metering pump speed.

[0039] (2) Adopt the method of passing nitrogen gas to make it hollow, and adjust the nitrogen flow rate of the nozzle to 0.1NI / min.

[0040] (3) During the spinning process, the mixed liquid composed of water and ethylene glycol at a weight ratio of 1:1 was used as a coagulation bath, and its temperature was adjusted to 60°C, and the receiving distance of the coagulation bath was 12cm.

[0041] (4) Soak the membrane filaments in ethanol at 60° C. for 48 hours, then soak them in distilled water for 24 hours, freeze-dry them and store them for later use. Through electron microscope analysis, ther...

Embodiment 2

[0043] (1) Batching (PPS: BP: BZ = 50%: 50%: 0%), crushed by a pulverizer and mixed evenly, set the heating temperature for each segment (225°C, 264°C, 265°C, 261°C, 260°C, 260°C), spinneret temperature and metering pump temperature (245°C, 245°C), after the temperature stabilizes, adjust the speed of the main engine, feeding speed and metering pump.

[0044] (2) Adopt the method of passing nitrogen gas to make it hollow, and adjust the nitrogen flow rate of the nozzle to 0.1NI / min.

[0045] (3) During the spinning process, the mixed liquid composed of water and ethylene glycol at a weight ratio of 1:1 was used as a coagulation bath, and its temperature was adjusted to 60°C, and the receiving distance of the coagulation bath was 12cm.

[0046] (4) Soak the membrane filaments in ethanol at 60° C. for 48 hours, then soak them in distilled water for 24 hours, freeze-dry them and store them for later use. Through electron microscope analysis, there are fine crystal particles in t...

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Abstract

The invention discloses a preparation method for a microporous polyphenylene sulfide hollow fiber membrane. The preparation method comprises the following steps of 1) uniformly mixing a diluent, a pore-forming agent, inorganic nanoparticles and polyphenylene sulfide so as to obtain a homogeneous-phase polyphenylene sulfide membrane casting solution; 2) adjusting the feeding rotating speed of a screw machine, the rotating speed of a main engine, the rotating speed of a metering pump and the heating temperature of each part, and then putting the polyphenylene sulfide membrane casting solution obtained in step 1) into the screw machine; 3) setting the gas flow rate or the core liquid flow rate of a nozzle of the screw machine, setting the temperature of a coagulating bath and the receiving distance of the coagulating bath, and carrying out spinning; and 4) immersing membrane yarns obtained in step 3) into a heated extraction agent, and carrying out drying to remove the organic solvent soas to obtain the microporous polyphenylene sulfide hollow fiber membrane. According to the method, the inorganic nanoparticles and the auxiliary diluent are added to regulate and control the crystallization rate and the phase-splitting process of the membrane casting solution; and the diluent is separated out by the aid of extraction liquid, and then the hollow fiber membrane with micro-nano through holes which are formed in the inner surface and the outer surface, enable the outside to be communicated with the inside and are uniformly distributed is obtained.

Description

technical field [0001] The invention relates to the field of polymer hollow fiber membrane preparation, in particular to a method for preparing a microporous polyphenylene sulfide hollow fiber membrane. Background technique [0002] Membrane separation technology, as a new type of high-efficiency separation technology, has been valued and recognized by countries all over the world, especially in the aspects of industrial energy saving, optimization and improvement of production process and efficiency, reuse of raw materials and environmental pollution control. more important effect. In recent years, membrane technology has developed rapidly and has been widely used in sewage treatment, seawater desalination, energy-saving technology, petrochemical pharmaceuticals, environment, electronics, energy and aerospace. However, the separation problem in some harsh environments is highlighted, especially the "corrosive waste liquid / waste gas treatment" in the fields of medicine, ene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/66B01D69/08B01D67/00
CPCB01D67/0002B01D69/08B01D71/66
Inventor 李振环高原程博闻
Owner TIANJIN POLYTECHNIC UNIV
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