阅读说明：本技术 一种石墨烯复合聚酯中空纤维膜及其制备方法 (Graphene composite polyester hollow fiber membrane and preparation method thereof ) 是由 任国峰 马立国 刘少华 于 2021-01-15 设计创作，主要内容包括：本发明公开了一种石墨烯复合聚酯中空纤维膜及其制备方法,该方法包含：制备石墨烯粉体；将石墨烯粉体与聚酯粉体混合,加入螺杆挤出机,制备复合聚酯母粒；将复合聚酯母粒与空白聚酯切片混合,加入纺丝机中,制备复合聚酯纤维；将复合聚酯纤维编制成中空纤维内衬管；浸入表面添加剂中；配置聚四氟乙烯中空纤维膜铸膜液；采用纺丝设备,将聚四氟乙烯铸膜液涂覆在石墨烯聚酯内衬管上,得到石墨烯聚酯中空纤维膜；浸入溶剂槽中；继续牵拉,并浸入水槽中,水槽中装有纯净水,去除多余的溶剂；牵拉缠绕在纺丝辊上,按照需求裁剪。本发明还提供了通过该方法制备的中空纤维膜。本发明制备的中空纤维膜具有机械强度好,耐水压大,抗菌性能优越等特点。(The invention discloses a graphene composite polyester hollow fiber membrane and a preparation method thereof, wherein the method comprises the following steps: preparing graphene powder; mixing graphene powder and polyester powder, adding the mixture into a screw extruder, and preparing composite polyester master batch; mixing the composite polyester master batch with the blank polyester chip, and adding the mixture into a spinning machine to prepare composite polyester fiber; weaving the composite polyester fiber into a hollow fiber lining pipe; immersing in a surface additive; preparing a polytetrafluoroethylene hollow fiber membrane casting solution; coating the polytetrafluoroethylene membrane casting solution on a graphene polyester lining pipe by adopting spinning equipment to obtain a graphene polyester hollow fiber membrane; immersing in a solvent bath; continuously drawing, and immersing into a water tank filled with purified water to remove redundant solvent; and (4) drawing and winding the yarn on a spinning roller, and cutting the yarn according to requirements. The invention also provides a hollow fiber membrane prepared by the method. The hollow fiber membrane prepared by the invention has the characteristics of good mechanical strength, high water pressure resistance, excellent antibacterial performance and the like.)

1. A preparation method of a graphene composite polyester hollow fiber membrane is characterized by comprising the following steps:

step 1, preparing graphene powder;

step 2, mixing the graphene powder and the polyester powder, adding the mixture into a screw extruder, and preparing the graphene composite polyester master batch;

step 3, adding the graphene composite polyester master batches and the blank polyester chips into a spinning machine to prepare the graphene composite polyester fiber;

step 4, weaving the graphene composite polyester fiber into a hollow tubular shape to obtain a hollow fiber lining pipe;

step 5, immersing the hollow fiber lining pipe into the surface additive;

step 6, preparing a polytetrafluoroethylene hollow fiber membrane casting solution;

step 7, uniformly coating the polytetrafluoroethylene membrane casting solution on a graphene polyester lining pipe by using spinning equipment to prepare a graphene polyester hollow fiber membrane;

step 8, immersing the graphene polyester hollow fiber membrane into a solvent tank;

step 9, continuously drawing the graphene polyester hollow fiber membrane, and immersing the graphene polyester hollow fiber membrane into a water tank to remove redundant solvent;

and step 10, drawing and winding the graphene composite polyester hollow fiber membrane on a spinning roller, and cutting according to the size requirement to obtain the required graphene composite polyester hollow fiber membrane.

2. The method for preparing the graphene composite polyester hollow fiber membrane according to claim 1, wherein in the step 1, graphene powder is prepared by an oxidation-reduction method.

3. The method for preparing the graphene composite polyester hollow fiber membrane according to claim 1, wherein in the step 2, the mixture of graphene powder and polyester powder comprises 5% -20% of graphene powder and 80% -95% of polyester powder by mass percent.

4. The preparation method of the graphene composite polyester hollow fiber membrane as claimed in claim 1, wherein in the step 3, the graphene composite polyester master batch and the blank polyester chip are mixed according to the mass ratio of (1:1) - (1:4), and are added into a spinning machine, the temperature is set to 240-260 ℃, the extrusion rate is 50-80 r/min, and the diameter range of the prepared graphene composite polyester fiber is 0.01-0.05 mm.

5. The method for preparing the graphene composite polyester hollow fiber membrane according to claim 1, wherein in the step 4, the graphene composite polyester fiber is knitted into a hollow tubular shape by a crocheting process and a 24-spindle high-speed knitting machine; the outer diameter of the hollow tube is 1.85-1.95mm, and the inner diameter is ≧ 1.2 mm.

6. The method for preparing the graphene composite polyester hollow fiber membrane according to claim 1, wherein in the step 5, the surface additive is a glycol solution with a mass concentration of 20% -40%.

7. The method for preparing the graphene composite polyester hollow fiber membrane according to claim 1, wherein in the step 7, the diameter of a spinning roller of a spinning device is 1.0-1.5 m, and the rotating speed is 5-10 r/min.

8. The method for preparing the graphene composite polyester hollow fiber membrane according to claim 1, wherein in the step 8, the graphene composite polyester hollow fiber membrane is immersed in a solvent tank, glycerol is filled in the solvent tank as a solvent, and the immersion time is 2-10 seconds.

9. The method for preparing the graphene composite polyester hollow fiber membrane according to claim 1, wherein in the step 9, purified water is filled in a water tank, the water temperature is 30-60 ℃, and the immersion time is 5-20 seconds.

10. A graphene composite polyester hollow fiber membrane prepared by the method of any one of claims 1 to 9.

Technical Field

The invention relates to a hollow fiber membrane and a preparation method thereof, in particular to a graphene composite polyester hollow fiber membrane and a preparation method thereof.

Background

The ultrafiltration membrane is widely applied to industrial pure water treatment and wastewater treatment, and the operation of the industrial ultrafiltration membrane is generally divided into internal pressure and external pressure.

The household ultrafiltration membrane (hollow fiber membrane) separation technology is one of the six high and new technologies in the twenty-first century, has become a standard of separation process by the remarkable characteristics of operation at normal temperature and low pressure, no phase change, low energy consumption and the like, and is widely used in developed countries and regions in Europe and America and the like. Ultrafiltration membranes have been widely used in many fields such as drinking mineral water purification, beverage food, medical medicine, etc.

The dissolved substances and substances having a smaller pore diameter than the membrane permeate the ultrafiltration membrane as a permeate, and the substances that do not permeate the filtration membrane are gradually concentrated in the effluent. The produced water (permeate) will thus contain water, ions, and small molecular weight species, while colloidal species, large molecular species, particles, bacteria, viruses, protozoa, etc. will be trapped by the membrane and removed by concentrated water discharge, backwash and chemical cleaning.

The aperture range of the industrial ultrafiltration membrane is about 0.01-0.1 um, and the industrial ultrafiltration membrane has a good effect of removing pollutants such as particulate matters, bacteria, viruses, colloids and macromolecular organic matters in a water body.

The ultrafiltration membrane has good mechanical strength and can bear higher water pressure and impact resistance.

The hollow fiber membrane is in a fibrous shape, is generally processed into hollow fiber filaments by taking polysulfone and dimethylacetamide as raw materials, and has a selective permeability characteristic by dividing the hollow fiber filaments by a high-permeability polymer. Generally, in a water purification system, the inner cavity of the membrane wire is hollow, and in an industrial membrane wire, the inner cavity of the membrane wire is provided with a polyester rope, so that the water pressure resistance can be enhanced.

Graphene (Graphene) is a two-dimensional carbon nanomaterial consisting of carbon atoms in a hexagonal honeycomb lattice with sp2 hybridized orbitals. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future.

Disclosure of Invention

The invention aims to provide a graphene hollow fiber membrane and a preparation method thereof.

In order to achieve the above object, the present invention provides a method for preparing a graphene composite polyester hollow fiber membrane, wherein the method comprises: step 1, preparing graphene powder; step 2, mixing the graphene powder and the polyester powder, adding the mixture into a screw extruder, and preparing the graphene composite polyester master batch; step 3, adding the graphene composite polyester master batches and the blank polyester chips into a spinning machine to prepare the graphene composite polyester fiber; step 4, weaving the graphene composite polyester fiber into a hollow tubular shape to obtain a hollow fiber lining pipe; step 5, immersing the hollow fiber lining pipe into the surface additive; step 6, preparing a polytetrafluoroethylene hollow fiber membrane casting solution; step 7, uniformly coating the polytetrafluoroethylene membrane casting solution on a graphene polyester lining pipe by using spinning equipment to prepare a graphene polyester hollow fiber membrane; step 8, immersing the graphene polyester hollow fiber membrane into a solvent tank; step 9, continuously drawing the graphene polyester hollow fiber membrane, and immersing the graphene polyester hollow fiber membrane into a water tank to remove redundant solvent; and step 10, drawing and winding the graphene composite polyester hollow fiber membrane on a spinning roller, and cutting according to the size requirement to obtain the required graphene composite polyester hollow fiber membrane.

In the preparation method of the graphene composite polyester hollow fiber membrane, in the step 1, graphene powder is prepared by an oxidation-reduction method.

In the preparation method of the graphene composite polyester hollow fiber membrane, in the step 2, the mixture of the graphene powder and the polyester powder comprises 5-20% of the graphene powder and 80-95% of the polyester powder by mass percent.

In the step 3, the graphene composite polyester master batch and the blank polyester chip are mixed according to the mass ratio of (1:1) - (1:4), and are added into a spinning machine, the temperature is set to 240-260 ℃, the extrusion rate is 50r/min-80r/min, and the diameter range of the prepared graphene composite polyester fiber is 0.01-0.05 mm.

In the step 4, the graphene composite polyester fiber is braided into a hollow tube shape by a crocheting process and a 24-spindle high-speed braiding machine; the outer diameter of the hollow tube is 1.85-1.95mm, and the inner diameter is ≧ 1.2 mm.

In the preparation method of the graphene composite polyester hollow fiber membrane, in the step 5, the surface additive is an ethylene glycol solution with a mass concentration of 20-40%.

In the step 7, the diameter of the spinning roller of the spinning equipment is 1.0-1.5 m, and the rotating speed is 5-10 r/min.

In the step 8, the graphene composite polyester hollow fiber membrane is immersed in a solvent tank, wherein glycerol is filled in the solvent tank as a solvent, and the immersion time is 2 to 10 seconds.

In the preparation method of the graphene composite polyester hollow fiber membrane, in the step 9, purified water is filled in a water tank, the water temperature is 30-60 ℃, and the immersion time is 5-20 seconds.

The invention also provides the graphene composite polyester hollow fiber membrane prepared by the method.

The graphene composite polyester hollow fiber membrane and the preparation method thereof provided by the invention have the following advantages:

according to the invention, the graphene is added into the polyester liner, so that the antibacterial property of the polyester liner is improved, the membrane pores are prevented from being blocked by bacteria, and the mechanical property strength of the membrane yarn, such as tensile resistance, water pressure resistance and the like, can be improved.

The graphene composite polyester hollow fiber membrane prepared by the invention has the characteristics of good mechanical strength, high water pressure resistance, excellent antibacterial performance and the like.

Detailed Description

The following further describes embodiments of the present invention.

The invention provides a preparation method of a graphene composite polyester hollow fiber membrane, which comprises the following steps: step 1, preparing graphene powder; step 2, mixing the graphene powder and the polyester powder, adding the mixture into a screw extruder, and preparing the graphene composite polyester master batch; step 3, adding the graphene composite polyester master batches and the blank polyester chips into a spinning machine to prepare the graphene composite polyester fiber; step 4, weaving the graphene composite polyester fiber into a hollow tubular shape to obtain a hollow fiber lining pipe; step 5, immersing the hollow fiber lining pipe into the surface additive; step 6, preparing a polytetrafluoroethylene hollow fiber membrane casting solution; step 7, uniformly coating the polytetrafluoroethylene membrane casting solution on a graphene polyester lining pipe by using spinning equipment to prepare a graphene polyester hollow fiber membrane; step 8, immersing the graphene polyester hollow fiber membrane into a solvent tank; step 9, continuously drawing the graphene polyester hollow fiber membrane, and immersing the graphene polyester hollow fiber membrane into a water tank to remove redundant solvent; and step 10, drawing and winding the graphene composite polyester hollow fiber membrane on a spinning roller, and cutting according to the size requirement to obtain the required graphene composite polyester hollow fiber membrane.

Preferably, in step 1, the graphene powder is prepared by a redox method.

In the step 2, the mixture of the graphene powder and the polyester powder comprises 5-20% of the graphene powder and 80-95% of the polyester powder by mass percent.

In the step 3, mixing the graphene composite polyester master batch and the blank polyester chip according to the mass ratio of (1:1) - (1:4), adding the mixture into a spinning machine, setting the temperature at 240-260 ℃, and the extrusion rate at 50-80 r/min, wherein the diameter range of the prepared graphene composite polyester fiber is 0.01-0.05 mm.

In the step 4, the graphene composite polyester fiber is woven into a hollow tubular shape by a crocheting process and a 24-spindle high-speed weaving machine; the outer diameter of the hollow tube is 1.85-1.95mm, and the inner diameter is ≧ 1.2 mm. The tube wall has uniform gaps, and has the characteristics of enhancing the toughness and strength of the membrane wire, prolonging the service life of the membrane wire and the like.

In step 5, the surface additive is an ethylene glycol solution with the mass concentration of 20-40%.

In the step 6, the polytetrafluoroethylene hollow fiber membrane casting solution comprises, by mass, 60% -80% of polytetrafluoroethylene, 5% -10% of a pore-forming agent, 8% -10% of a plasticizer, 5% -10% of a toughening agent, 2% -20% of an auxiliary additive and the like. The pore-foaming agent, the plasticizer, the toughening agent, the auxiliary additive and the like are all chemical preparations existing in the field.

In step 7, the diameter of a spinning roller of the spinning equipment is 1.0-1.5 m, and the rotating speed is 5-10 r/min.

And 8, immersing the graphene polyester hollow fiber membrane into a solvent tank, wherein glycerol is filled in the solvent tank to serve as a solvent, and the immersion time is 2-10 seconds.

In step 9, the water tank is filled with purified water, the water temperature is 30-60 ℃, and the immersion time is 5-20 seconds.

The invention also provides the graphene composite polyester hollow fiber membrane prepared by the method.

The graphene composite polyester hollow fiber membrane and the preparation method thereof provided by the invention are further described below with reference to the examples.

Example 1

A preparation method of a graphene composite polyester hollow fiber membrane comprises the following steps:

step 1, preparing graphene powder.

Preferably, the graphene powder is prepared by a redox method.

And 2, mixing the graphene powder and the polyester powder, adding the mixture into a screw extruder, and preparing the graphene composite polyester master batch.

The mixture of the graphene powder and the polyester powder comprises 5% of the graphene powder and 95% of the polyester powder by mass percent.

And 3, mixing the graphene composite polyester master batch and the blank polyester chip according to a certain proportion, adding the mixture into a spinning machine, and setting the temperature and the extrusion rate to prepare the graphene composite polyester fiber.

Mixing the graphene composite polyester master batch and the blank polyester chip according to the mass ratio of 1:1, adding the mixture into a spinning machine, setting the temperature at 240-260 ℃, and the extrusion rate at 50-80 r/min, thereby preparing the graphene composite polyester fiber.

The diameter range of the graphene composite polyester fiber is 0.01-0.05 mm.

And 4, weaving the graphene composite polyester fibers into a hollow tubular shape according to a certain standard to obtain the hollow fiber lining pipe.

Weaving the graphene composite polyester fiber into a hollow tubular shape by a crocheting process and a 24-spindle high-speed braiding machine; the outer diameter of the hollow tube is 1.85-1.95mm, and the inner diameter is ≧ 1.2 mm. The tube wall has uniform gaps, and has the characteristics of enhancing the toughness and strength of the membrane wire, prolonging the service life of the membrane wire and the like.

And 5, immersing the hollow fiber lining pipe into the surface additive. The surface additive is ethylene glycol solution with mass concentration of 20%.

And 6, preparing a polytetrafluoroethylene hollow fiber membrane casting solution.

The polytetrafluoroethylene hollow fiber membrane casting solution comprises, by mass, 60% of polytetrafluoroethylene, 10% of a pore-forming agent, 10% of a plasticizer, 10% of a toughening agent, 10% of an auxiliary additive and the like. The pore-foaming agent, the plasticizer, the toughening agent, the auxiliary additive and the like are all chemical preparations existing in the field.

And 7, setting the rotating speed of a spinning roller and the spinning speed of the casting solution in a spinning nozzle by adopting spinning equipment, and uniformly coating the polytetrafluoroethylene casting solution on the graphene polyester lining pipe to prepare the graphene polyester hollow fiber membrane. The diameter of the spinning roller of the spinning equipment is 1.0-1.5 m, and the rotating speed is 5-10 r/min.

And 8, immersing the graphene polyester hollow fiber membrane into a solvent tank, wherein glycerol is filled in the solvent tank to serve as a solvent, and the immersion time is 2-10 seconds.

And 9, continuously drawing the graphene polyester hollow fiber membrane, and immersing the graphene polyester hollow fiber membrane into a water tank, wherein purified water is filled in the water tank, the water temperature is 30-60 ℃, and the immersion time is 5-20 seconds, and the graphene polyester hollow fiber membrane is used for removing redundant solvents.

And step 10, drawing and winding the graphene composite polyester hollow fiber membrane on a spinning roller, and cutting according to the size requirement to obtain the required graphene composite polyester hollow fiber membrane.

The embodiment also provides the graphene composite polyester hollow fiber membrane prepared by the method.

Example 2

A preparation method of a graphene composite polyester hollow fiber membrane comprises the following steps:

step 1, preparing graphene powder.

Preferably, the graphene powder is prepared by a redox method.

And 2, mixing the graphene powder and the polyester powder, adding the mixture into a screw extruder, and preparing the graphene composite polyester master batch.

The mixture of the graphene powder and the polyester powder comprises 10% of the graphene powder and 90% of the polyester powder by mass percent.

And 3, mixing the graphene composite polyester master batch and the blank polyester chip according to a certain proportion, adding the mixture into a spinning machine, and setting the temperature and the extrusion rate to prepare the graphene composite polyester fiber.

Mixing the graphene composite polyester master batch and the blank polyester chip according to the mass ratio of 1:1.5, adding the mixture into a spinning machine, setting the temperature at 240-260 ℃, and the extrusion rate at 50-80 r/min, thereby preparing the graphene composite polyester fiber.

The diameter range of the graphene composite polyester fiber is 0.01-0.05 mm.

And 4, weaving the graphene composite polyester fibers into a hollow tubular shape according to a certain standard to obtain the hollow fiber lining pipe.

Weaving the graphene composite polyester fiber into a hollow tubular shape by a crocheting process and a 24-spindle high-speed braiding machine; the outer diameter of the hollow tube is 1.85-1.95mm, and the inner diameter is ≧ 1.2 mm. The tube wall has uniform gaps, and has the characteristics of enhancing the toughness and strength of the membrane wire, prolonging the service life of the membrane wire and the like.

And 5, immersing the hollow fiber lining pipe into the surface additive. The surface additive is ethylene glycol solution with the mass concentration of 25%.

And 6, preparing a polytetrafluoroethylene hollow fiber membrane casting solution.

The polytetrafluoroethylene hollow fiber membrane casting solution comprises 62% of polytetrafluoroethylene, 5% of pore-forming agent, 8% of plasticizer, 5% of toughening agent, 20% of auxiliary additive and the like according to mass percentage. The pore-foaming agent, the plasticizer, the toughening agent, the auxiliary additive and the like are all chemical preparations existing in the field.

And 7, setting the rotating speed of a spinning roller and the spinning speed of the casting solution in a spinning nozzle by adopting spinning equipment, and uniformly coating the polytetrafluoroethylene casting solution on the graphene polyester lining pipe to prepare the graphene polyester hollow fiber membrane. The diameter of the spinning roller of the spinning equipment is 1.0-1.5 m, and the rotating speed is 5-10 r/min.

And 8, immersing the graphene polyester hollow fiber membrane into a solvent tank, wherein glycerol is filled in the solvent tank to serve as a solvent, and the immersion time is 2-10 seconds.

And 9, continuously drawing the graphene polyester hollow fiber membrane, and immersing the graphene polyester hollow fiber membrane into a water tank, wherein purified water is filled in the water tank, the water temperature is 30-60 ℃, and the immersion time is 5-20 seconds, and the graphene polyester hollow fiber membrane is used for removing redundant solvents.

And step 10, drawing and winding the graphene composite polyester hollow fiber membrane on a spinning roller, and cutting according to the size requirement to obtain the required graphene composite polyester hollow fiber membrane.

The embodiment also provides the graphene composite polyester hollow fiber membrane prepared by the method.

Example 3

A preparation method of a graphene composite polyester hollow fiber membrane comprises the following steps:

step 1, preparing graphene powder.

Preferably, the graphene powder is prepared by a redox method.

And 2, mixing the graphene powder and the polyester powder, adding the mixture into a screw extruder, and preparing the graphene composite polyester master batch.

The mixture of the graphene powder and the polyester powder comprises 12% of the graphene powder and 88% of the polyester powder by mass percent.

And 3, mixing the graphene composite polyester master batch and the blank polyester chip according to a certain proportion, adding the mixture into a spinning machine, and setting the temperature and the extrusion rate to prepare the graphene composite polyester fiber.

Mixing the graphene composite polyester master batch and the blank polyester chip according to the mass ratio of 1:2, adding the mixture into a spinning machine, setting the temperature at 240-260 ℃, and the extrusion rate at 50-80 r/min, thereby preparing the graphene composite polyester fiber.

The diameter range of the graphene composite polyester fiber is 0.01-0.05 mm.

And 4, weaving the graphene composite polyester fibers into a hollow tubular shape according to a certain standard to obtain the hollow fiber lining pipe.

Weaving the graphene composite polyester fiber into a hollow tubular shape by a crocheting process and a 24-spindle high-speed braiding machine; the outer diameter of the hollow tube is 1.85-1.95mm, and the inner diameter is ≧ 1.2 mm. The tube wall has uniform gaps, and has the characteristics of enhancing the toughness and strength of the membrane wire, prolonging the service life of the membrane wire and the like.

And 5, immersing the hollow fiber lining pipe into the surface additive. The surface additive is ethylene glycol solution with the mass concentration of 30%.

And 6, preparing a polytetrafluoroethylene hollow fiber membrane casting solution.

The polytetrafluoroethylene hollow fiber membrane casting solution comprises 64% of polytetrafluoroethylene, 6% of pore-forming agent, 9% of plasticizer, 6% of toughening agent, 15% of auxiliary additive and the like according to mass percentage. The pore-foaming agent, the plasticizer, the toughening agent, the auxiliary additive and the like are all chemical preparations existing in the field.

And 7, setting the rotating speed of a spinning roller and the spinning speed of the casting solution in a spinning nozzle by adopting spinning equipment, and uniformly coating the polytetrafluoroethylene casting solution on the graphene polyester lining pipe to prepare the graphene polyester hollow fiber membrane. The diameter of the spinning roller of the spinning equipment is 1.0-1.5 m, and the rotating speed is 5-10 r/min.

And 8, immersing the graphene polyester hollow fiber membrane into a solvent tank, wherein glycerol is filled in the solvent tank to serve as a solvent, and the immersion time is 2-10 seconds.

And 9, continuously drawing the graphene polyester hollow fiber membrane, and immersing the graphene polyester hollow fiber membrane into a water tank, wherein purified water is filled in the water tank, the water temperature is 30-60 ℃, and the immersion time is 5-20 seconds, and the graphene polyester hollow fiber membrane is used for removing redundant solvents.

And step 10, drawing and winding the graphene composite polyester hollow fiber membrane on a spinning roller, and cutting according to the size requirement to obtain the required graphene composite polyester hollow fiber membrane.

The embodiment also provides the graphene composite polyester hollow fiber membrane prepared by the method.

Example 4

A preparation method of a graphene composite polyester hollow fiber membrane comprises the following steps:

a preparation method of a graphene composite polyester hollow fiber membrane comprises the following steps:

step 1, preparing graphene powder.

Preferably, the graphene powder is prepared by a redox method.

And 2, mixing the graphene powder and the polyester powder, adding the mixture into a screw extruder, and preparing the graphene composite polyester master batch.

The mixture of the graphene powder and the polyester powder comprises 18% of the graphene powder and 82% of the polyester powder in percentage by mass.

And 3, mixing the graphene composite polyester master batch and the blank polyester chip according to a certain proportion, adding the mixture into a spinning machine, and setting the temperature and the extrusion rate to prepare the graphene composite polyester fiber.

Mixing the graphene composite polyester master batch and the blank polyester chip according to the mass ratio of 1:3, adding the mixture into a spinning machine, setting the temperature at 240-260 ℃, and the extrusion rate at 50-80 r/min, thereby preparing the graphene composite polyester fiber.

The diameter range of the graphene composite polyester fiber is 0.01-0.05 mm.

And 4, weaving the graphene composite polyester fibers into a hollow tubular shape according to a certain standard to obtain the hollow fiber lining pipe.

Weaving the graphene composite polyester fiber into a hollow tubular shape by a crocheting process and a 24-spindle high-speed braiding machine; the outer diameter of the hollow tube is 1.85-1.95mm, and the inner diameter is ≧ 1.2 mm. The tube wall has uniform gaps, and has the characteristics of enhancing the toughness and strength of the membrane wire, prolonging the service life of the membrane wire and the like.

And 5, immersing the hollow fiber lining pipe into the surface additive. The surface additive is ethylene glycol solution with mass concentration of 35%.

And 6, preparing a polytetrafluoroethylene hollow fiber membrane casting solution.

The polytetrafluoroethylene hollow fiber membrane casting solution comprises, by mass, 70.5% of polytetrafluoroethylene, 8% of a pore-forming agent, 8.5% of a plasticizer, 8% of a toughening agent, 5% of an auxiliary additive and the like. The pore-foaming agent, the plasticizer, the toughening agent, the auxiliary additive and the like are all chemical preparations existing in the field.

And 7, setting the rotating speed of a spinning roller and the spinning speed of the casting solution in a spinning nozzle by adopting spinning equipment, and uniformly coating the polytetrafluoroethylene casting solution on the graphene polyester lining pipe to prepare the graphene polyester hollow fiber membrane. The diameter of the spinning roller of the spinning equipment is 1.0-1.5 m, and the rotating speed is 5-10 r/min.

And 8, immersing the graphene polyester hollow fiber membrane into a solvent tank, wherein glycerol is filled in the solvent tank to serve as a solvent, and the immersion time is 2-10 seconds.

And 9, continuously drawing the graphene polyester hollow fiber membrane, and immersing the graphene polyester hollow fiber membrane into a water tank, wherein purified water is filled in the water tank, the water temperature is 30-60 ℃, and the immersion time is 5-20 seconds, and the graphene polyester hollow fiber membrane is used for removing redundant solvents.

And step 10, drawing and winding the graphene composite polyester hollow fiber membrane on a spinning roller, and cutting according to the size requirement to obtain the required graphene composite polyester hollow fiber membrane.

The embodiment also provides the graphene composite polyester hollow fiber membrane prepared by the method.

Example 5

A preparation method of a graphene composite polyester hollow fiber membrane comprises the following steps:

step 1, preparing graphene powder.

Preferably, the graphene powder is prepared by a redox method.

And 2, mixing the graphene powder and the polyester powder, adding the mixture into a screw extruder, and preparing the graphene composite polyester master batch.

The mixture of the graphene powder and the polyester powder comprises 20% of the graphene powder and 80% of the polyester powder by mass percent.

And 3, mixing the graphene composite polyester master batch and the blank polyester chip according to a certain proportion, adding the mixture into a spinning machine, and setting the temperature and the extrusion rate to prepare the graphene composite polyester fiber.

Mixing the graphene composite polyester master batch and the blank polyester chip according to the mass ratio of 1:4, adding the mixture into a spinning machine, setting the temperature at 240-260 ℃, and the extrusion rate at 50-80 r/min, thereby preparing the graphene composite polyester fiber.

The diameter range of the graphene composite polyester fiber is 0.01-0.05 mm.

And 4, weaving the graphene composite polyester fibers into a hollow tubular shape according to a certain standard to obtain the hollow fiber lining pipe.

Weaving the graphene composite polyester fiber into a hollow tubular shape by a crocheting process and a 24-spindle high-speed braiding machine; the outer diameter of the hollow tube is 1.85-1.95mm, and the inner diameter is ≧ 1.2 mm. The tube wall has uniform gaps, and has the characteristics of enhancing the toughness and strength of the membrane wire, prolonging the service life of the membrane wire and the like.

And 5, immersing the hollow fiber lining pipe into the surface additive. The surface additive is glycol solution with mass concentration of 40%.

And 6, preparing a polytetrafluoroethylene hollow fiber membrane casting solution.

The polytetrafluoroethylene hollow fiber membrane casting solution comprises, by mass, 80% of polytetrafluoroethylene, 5% of a pore-forming agent, 8% of a plasticizer, 5% of a toughening agent, 2% of an auxiliary additive and the like. The pore-foaming agent, the plasticizer, the toughening agent, the auxiliary additive and the like are all chemical preparations existing in the field.

And 7, setting the rotating speed of a spinning roller and the spinning speed of the casting solution in a spinning nozzle by adopting spinning equipment, and uniformly coating the polytetrafluoroethylene casting solution on the graphene polyester lining pipe to prepare the graphene polyester hollow fiber membrane. The diameter of the spinning roller of the spinning equipment is 1.0-1.5 m, and the rotating speed is 5-10 r/min.

And 8, immersing the graphene polyester hollow fiber membrane into a solvent tank, wherein glycerol is filled in the solvent tank to serve as a solvent, and the immersion time is 2-10 seconds.

And 9, continuously drawing the graphene polyester hollow fiber membrane, and immersing the graphene polyester hollow fiber membrane into a water tank, wherein purified water is filled in the water tank, the water temperature is 30-60 ℃, and the immersion time is 5-20 seconds, and the graphene polyester hollow fiber membrane is used for removing redundant solvents.

And step 10, drawing and winding the graphene composite polyester hollow fiber membrane on a spinning roller, and cutting according to the size requirement to obtain the required graphene composite polyester hollow fiber membrane.

The embodiment also provides the graphene composite polyester hollow fiber membrane prepared by the method.

The graphene composite polyester hollow fiber membrane and the preparation method thereof provided by the invention are mainly characterized in that graphene is added into a polyester lining, so that the antibacterial property of the lining is enhanced, the membrane pores are prevented from being blocked by bacteria residue, and in addition, the mechanical strength of the hollow fiber is increased by the graphene polyester.

While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.