CN110523298A - A kind of enhanced polyethylene hollow fiber membrane and preparation method thereof - Google Patents

A kind of enhanced polyethylene hollow fiber membrane and preparation method thereof Download PDF

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Publication number
CN110523298A
CN110523298A CN201810517141.9A CN201810517141A CN110523298A CN 110523298 A CN110523298 A CN 110523298A CN 201810517141 A CN201810517141 A CN 201810517141A CN 110523298 A CN110523298 A CN 110523298A
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China
Prior art keywords
hollow fiber
fiber membrane
enhanced polyethylene
film
polyethylene
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Application number
CN201810517141.9A
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Chinese (zh)
Inventor
傅寅翼
吴低潮
王鑫臻
黄江益
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Ningbo Jingyuan Environmental Development Co Ltd
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Ningbo Jingyuan Environmental Development Co Ltd
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Priority to CN201810517141.9A priority Critical patent/CN110523298A/en
Publication of CN110523298A publication Critical patent/CN110523298A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0079—Manufacture of membranes comprising organic and inorganic components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/08—Hollow fibre membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/30—Polyalkenyl halides
    • B01D71/32—Polyalkenyl halides containing fluorine atoms
    • B01D71/34—Polyvinylidene fluoride
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/24—Mechanical properties, e.g. strength

Abstract

The invention discloses a kind of enhanced polyethylene hollow fiber membranes, are made of the film forming system of following mass ratio: polyethylene 20~45%；Graphene oxide 1~5%；Composite coupler 0.02~0.5%；Hydrophilic agent 1~25%；Diluent 30~70%；Pore former 2~20%.The invention also discloses a kind of preparation methods of enhanced polyethylene hollow fiber membrane, including each raw material mixed at high speed is prepared film forming material, then film forming material is cut into 7~50 millimeters of fillet through cutting machine, then fillet is sent into Wiring apparatus, it is wrapped on organic fiber pipe, hollow fiber conduit is obtained, then hollow fiber conduit is removed into diluent and pore former through gas phase or liquid phase separation, then obtain enhanced polyethylene hollow fiber membrane through low-temperature sintering.

Description

A kind of enhanced polyethylene hollow fiber membrane and preparation method thereof
Technical field
The present invention relates to technical field of composite materials, more specifically, it relates to a kind of enhanced polyethylene hollow fiber Film and preparation method thereof.
Background technique
In terms of water prevention and cure of pollution and the recycling and reusing of water resource, compared with tradition AO method, membrane bioreactor (MBR) be a kind of efficient water resource reuse and sewage treatment method.Core original part in membrane bioreactor is at sewage Reason filter membrane mainly includes curtain type membrane, plate membrane, tubular membrane, rolled film etc..Wherein curtain type membrane mainly uses doughnut Filter membrane is as filtering material.
For polyethylene as a kind of general-purpose plastics, yield is big and cheap, be the plastics that are most widely used at present it One.If its surcharge can not only can be greatly improved polythene material functionalization, but also its application neck can also be expanded Domain.Polyethylene hollow fiber microporous barrier is exactly this kind of material, has just been rapidly developed since 1970s come out, Application field is also constantly expanding, and is applied widely in industries such as water process, biomedicine, pharmacy, chemical industry and food.
Existing polyethylene hollow fiber microporous barrier mechanical strength is inadequate, and tensile resistance is poor, has seriously affected polyethylene The use of hollow-fibre membrane.
Summary of the invention
The object of the present invention is to provide a kind of high mechanical strength, the good enhanced polyethylene hollow fiber of tensile resistance Film improves the utilization rate of the film.
To achieve the above object, realized by following technological means: a kind of enhanced polyethylene hollow fiber membrane, by with The film forming system of lower mass ratio forms:
It advanced optimizes are as follows: the composite coupler is mixed by the silane coupling agent and titanate coupling agent of equal mass ratioes It forms.
It advanced optimizes are as follows: the hydrophilic agent is polyvinylpyrrolidone or polyethylene glycol.
Advanced optimize are as follows: the diluent be dibutyl phthalate, dioctyl phthalate, paraxylene, One of tributyl phosphate, tetrahydrofuran or a variety of combinations.
It advanced optimizes are as follows: the pore former is sodium chloride or lithium chloride or calcium chloride or calcium carbonate.
It is a further object of the present invention to provide a kind of preparation method of enhanced polyethylene hollow fiber membrane, including it is as follows Specific steps:
1) by polyethylene and graphene oxide, iron powder, composite coupler mixed at high speed；
2) hydrophilic agent, pore former, diluent are sequentially added in the ingredient after Xiang Shangshu mixed at high speed, is uniformly mixed system Film forming material；
3) above-mentioned film forming material is put into the fillet that cutting machine is cut into 7~50 millimeters, fillet is then sent into Wiring apparatus, It is wrapped on organic fiber pipe, obtains hollow fiber conduit；
4) compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then by hollow fiber conduit It is sent into gas phase or liquid phase separation slot, diluent, the pore former in film material is separated, PE hollow fiber film thread is obtained；
5) PE hollow fiber film thread is sent into drying tunnel and is sintered 10~60 seconds in 100~130 DEG C to get in enhancing polyethylene Empty fiber membrane.
It advanced optimizes are as follows: the winding layer number in the step 3) is no more than 10 layers.
It advanced optimizes are as follows: the organic fiber shell material in the step 3) is aramid fiber, polyether-ether-ketone, PSA fiber, gathers Poly P phenylene diamine terephthalamide, Visil fiber, polybenzimidazoles, polyphenylene sulfide or polyimides, sleeve outer 1-5.5 milli Rice, 0.5-4.5 millimeters of internal diameter.
Compared with prior art, the invention has the benefit that graphene oxide composite coupler and iron powder catalysis Under effect, branch occurs with matrix polythene material and connects, so that polyethylene fibre is linked to be net by graphene oxide branch, it is netted Structure increases the mechanical strength of polyethylene film, and gained film layer is not easily damaged, and resistance to physical damage ability is significantly increased；Poly- second Alkene is cheap, and graphene oxide is cheap and easy to get, prepares enhanced polyethylene hollow fiber membrane institute through graphene oxide enhancing It is at low cost to obtain film, it is cheap and easy to get.PE will form lamellar structure in fiber under stress field action during melt spinning, warp Up to PE hard elastic fibre after heat treatment, (spinning is led with spinning drawing ratio for the crystallinity and elastic recovery rate of PE hard elastic fibre Stretch ratio=winding rate/rate of extrusion) increase and increase, orientation and row of the high spinning drawing than being conducive to PE strand Column, promote platelet arranged in parallel to be formed, and the present invention uses the hollow fibre of enhanced polyethylene of high-temperature fusion high-speed stretch preparation The elastic recovery rate for tieing up film is high, and tensile resistance is strong, not fracture of wire.It please be described in detail and polyethylene hollow fiber membrane is prepared using winding method The advantages of, it preferably writes out to mechanical strength, the raising principle of tensile property.
Specific embodiment
Invention is described in further detail below by specific embodiment, it is not to limit that following embodiment, which is descriptive, Protection scope of the present invention of property.
Embodiment 1
A kind of enhanced polyethylene hollow fiber membrane is made of the film forming system of following mass ratio:
The composite coupler is mixed by the silane coupling agent and titanate coupling agent of equal mass ratioes.
The hydrophilic agent is polyvinylpyrrolidone.
The diluent is dibutyl phthalate.
The pore former is sodium chloride.
The preparation of the enhanced polyethylene hollow fiber membrane includes the following steps:
1) by polyethylene and graphene oxide, iron powder, composite coupler mixed at high speed；
2) hydrophilic agent, pore former, diluent are sequentially added in the ingredient after Xiang Shangshu mixed at high speed, is uniformly mixed system Film forming material；
3) above-mentioned film forming material is put into the fillet that cutting machine is cut into 7 millimeters, fillet is then sent into Wiring apparatus, wound On organic fiber pipe, hollow fiber conduit is obtained；The organic fiber pipe selection PSA fiber casing, outer diameter 3mm, internal diameter 1.8mm, Winding layer number is 2 layers；
4) compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then by hollow fiber conduit It is sent into gas phase or liquid phase separation slot, diluent, the pore former in film material is separated, PE hollow fiber film thread is obtained；
5) PE hollow fiber film thread is sent into drying tunnel and is sintered 10 seconds in 100 DEG C to get enhancing polyethylene hollow fiber membrane.
Embodiment 2
A kind of enhanced polyethylene hollow fiber membrane is made of the film forming system of following mass ratio:
The composite coupler is mixed by the silane coupling agent and titanate coupling agent of equal mass ratioes.
The hydrophilic agent is polyethylene glycol.
The diluent is dioctyl phthalate.
The pore former is lithium chloride.
The preparation of the enhanced polyethylene hollow fiber membrane includes the following steps:
1) by polyethylene and graphene oxide, iron powder, composite coupler mixed at high speed；
2) hydrophilic agent, pore former, diluent are sequentially added in the ingredient after Xiang Shangshu mixed at high speed, is uniformly mixed system Film forming material；
3) above-mentioned film forming material is put into the fillet that cutting machine is cut into 15 millimeters, fillet is then sent into Wiring apparatus, wound On organic fiber pipe, hollow fiber conduit is obtained；The organic fiber pipe uses polyether-ether-ketone casing, outer diameter 1.5mm, internal diameter 0.5mm, winding layer number are 4 layers；
4) compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then by hollow fiber conduit It is sent into gas phase or liquid phase separation slot, diluent, the pore former in film material is separated, PE hollow fiber film thread is obtained；
5) PE hollow fiber film thread is sent into drying tunnel and is sintered 12 seconds in 105 DEG C to get enhancing polyethylene hollow fiber membrane.
Embodiment 3
A kind of enhanced polyethylene hollow fiber membrane is made of the film forming system of following mass ratio:
The composite coupler is mixed by the silane coupling agent and titanate coupling agent of equal mass ratioes.
The hydrophilic agent is polyvinylpyrrolidone.
The diluent is paraxylene.
The pore former is calcium chloride.
The preparation of the enhanced polyethylene hollow fiber membrane includes the following steps:
1) by polyethylene and graphene oxide, iron powder, composite coupler mixed at high speed；
2) hydrophilic agent, pore former, diluent are sequentially added in the ingredient after Xiang Shangshu mixed at high speed, is uniformly mixed system Film forming material；
3) above-mentioned film forming material is put into the fillet that cutting machine is cut into 7~50 millimeters, fillet is then sent into Wiring apparatus, It is wrapped on organic fiber pipe, obtains hollow fiber conduit；The hollow fiber conduit selects poly(p-phenylene terephthalamide) casing, Outer diameter is 3.5mm, and internal diameter 2mm, winding layer number is 3 layers；
4) compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then by hollow fiber conduit It is sent into gas phase or liquid phase separation slot, diluent, the pore former in film material is separated, PE hollow fiber film thread is obtained；
5) PE hollow fiber film thread is sent into drying tunnel and is sintered 20 seconds in 110 DEG C to get enhancing polyethylene hollow fiber membrane.
Embodiment 4
A kind of enhanced polyethylene hollow fiber membrane is made of the film forming system of following mass ratio:
The composite coupler is mixed by the silane coupling agent and titanate coupling agent of equal mass ratioes.
The hydrophilic agent is polyethylene glycol.
The diluent is tributyl phosphate.
The pore former is calcium carbonate.
The preparation of the enhanced polyethylene hollow fiber membrane includes the following steps:
1) by polyethylene and graphene oxide, iron powder, composite coupler mixed at high speed；
2) hydrophilic agent, pore former, diluent are sequentially added in the ingredient after Xiang Shangshu mixed at high speed, is uniformly mixed system Film forming material；
3) above-mentioned film forming material is put into the fillet that cutting machine is cut into 7~50 millimeters, fillet is then sent into Wiring apparatus, It is wrapped on organic fiber pipe, obtains hollow fiber conduit；The organic fiber pipe selects Visil fiber sleeve, outer diameter 5mm, internal diameter 3mm, 5 layers of winding layer number；
4) compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then by hollow fiber conduit It is sent into gas phase or liquid phase separation slot, diluent, the pore former in film material is separated, PE hollow fiber film thread is obtained；
5) PE hollow fiber film thread is sent into drying tunnel and is sintered 30 seconds in 115 DEG C to get enhancing polyethylene hollow fiber membrane.
Embodiment 5
A kind of enhanced polyethylene hollow fiber membrane is made of the film forming system of following mass ratio:
The composite coupler is mixed by the silane coupling agent and titanate coupling agent of equal mass ratioes.
The hydrophilic agent is polyvinylpyrrolidone.
The diluent is tetrahydrofuran.
The pore former is sodium chloride.
The preparation of the enhanced polyethylene hollow fiber membrane includes the following steps:
1) by polyethylene and graphene oxide, iron powder, composite coupler mixed at high speed；
2) hydrophilic agent, pore former, diluent are sequentially added in the ingredient after Xiang Shangshu mixed at high speed, is uniformly mixed system Film forming material；
3) above-mentioned film forming material is put into the fillet that cutting machine is cut into 7~50 millimeters, fillet is then sent into Wiring apparatus, It is wrapped on organic fiber pipe, obtains hollow fiber conduit；The organic fiber pipe selects polyphenylene sulfide casing, outer diameter 4mm, interior Diameter is 1.8mm, and winding layer number is 6 layers；
4) compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then by hollow fiber conduit It is sent into gas phase or liquid phase separation slot, diluent, the pore former in film material is separated, PE hollow fiber film thread is obtained；
5) PE hollow fiber film thread is sent into drying tunnel and is sintered 40 seconds in 120 DEG C to get enhancing polyethylene hollow fiber membrane.
Comparative example
A kind of existing polyethylene hollow fiber membrane is made of the film forming system of following mass ratio:
The composite coupler is mixed by the silane coupling agent and titanate coupling agent of equal mass ratioes.
The hydrophilic agent is polyvinylpyrrolidone.
The diluent is tetrahydrofuran.
The pore former is sodium chloride.
The preparation of the existing polyethylene hollow fiber membrane includes the following steps:
1) by polyethylene and iron powder, composite coupler mixed at high speed；
2) hydrophilic agent, pore former, diluent are sequentially added in the ingredient after Xiang Shangshu mixed at high speed, is uniformly mixed system Film forming material；
3) above-mentioned film forming material is put into the fillet that cutting machine is cut into 50 millimeters, fillet is then sent into Wiring apparatus, wound On organic fiber pipe, hollow fiber conduit is obtained；The organic fiber pipe selects polyimides casing, outer diameter 5.5mm, internal diameter 3.2mm, winding layer number are 8 layers；
4) compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then by hollow fiber conduit It is sent into gas phase or liquid phase separation slot, diluent, the pore former in film material is separated, PE hollow fiber film thread is obtained；
5) PE hollow fiber film thread is sent into drying tunnel and is sintered 60 seconds in 130 DEG C to get enhancing polyethylene hollow fiber membrane.
Product obtained in above-described embodiment is tested for the property, test result is shown in Table 1:
Embodiment Pure water flux (LMH) Porosity % Elastic recovery rate % Scratch-resistant
Embodiment 1 2000 93 74 It is very strong
Embodiment 2 1900 90 75 It is very strong
Embodiment 3 2200 95 73 It is very strong
Embodiment 4 1800 88 76 It is very strong
Embodiment 5 2000 93 74 It is very strong
Comparative example 1300 72 59 Difference
In test process, the test of elastic recovery rate answers the stress-of sample with Japanese Shimadzu AG-1 type electric power puller system Become recovery curve to be tested, rate of extension 120mm/min, draft temperature is 25 DEG C, and sample initial length is 100mm, the calculation formula of elastic recovery rate (ER, %) are as follows: ER%=(l-l0)/(l’-l0) × 100%, l0To stretch preceding examination The length (mm) of sample, l are the length (mm) of sample after stretching, and l ' is the length (mm) of sample after replying.Scraping and wiping resistance performance is surveyed Method for testing is with coarse plastic friction wheel in the mantle friction identical time of hollow-fibre membrane, and observing hollow-fibre membrane is No destruction.
From test data as can be seen that the polyethylene hollow fiber membrane enhanced through graphene oxide is than not compound peroxide The existing polyethylene hollow fiber membrane of graphite alkene has better porosity, elastic recovery rate and scratch resistance, and elasticity is returned Multiple rate is higher, and the tensile property of tunica fibrosa is more preferable, improves the application performance of film.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned reality Example is applied, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for this technology For the those of ordinary skill in field, several improvements and modifications without departing from the principles of the present invention, these are improved and profit Decorations also should be regarded as protection scope of the present invention.

Claims (8)

1. a kind of enhanced polyethylene hollow fiber membrane, which is characterized in that be made of the film forming system of following mass ratio:
2. a kind of enhanced polyethylene hollow fiber membrane according to claim 1, which is characterized in that the composite coupler It is mixed by the silane coupling agent and titanate coupling agent of equal mass ratioes.
3. a kind of enhanced polyethylene hollow fiber membrane according to claim 1, which is characterized in that the hydrophilic agent is poly- Vinylpyrrolidone or polyethylene glycol.
4. a kind of enhanced polyethylene hollow fiber membrane according to claim 1, which is characterized in that the diluent is neighbour One of dibatyl phithalate, dioctyl phthalate, paraxylene, tributyl phosphate, tetrahydrofuran are a variety of Combination.
5. a kind of enhanced polyethylene hollow fiber membrane according to claim 1, which is characterized in that the pore former is chlorine Change sodium or lithium chloride or calcium chloride or calcium carbonate.
6. a kind of preparation method of enhanced polyethylene hollow fiber membrane, which is characterized in that comprise the following specific steps that:
1) by polyethylene and graphene oxide, iron powder, composite coupler mixed at high speed；
2) hydrophilic agent, pore former, diluent are sequentially added in the ingredient after Xiang Shangshu mixed at high speed, is uniformly mixed and film is made Material；
3) above-mentioned film forming material is put into the fillet that cutting machine is cut into 7~50 millimeters, fillet is then sent into Wiring apparatus, be wrapped in On organic fiber pipe, hollow fiber conduit is obtained；
4) it is passed through compressed air or higher boiling non-solvent into hollow fiber conduit as core liquid, hollow fiber conduit is then sent into gas Mutually or in liquid phase separation slot, diluent, the pore former in film material are separated, PE hollow fiber film thread is obtained；
5) PE hollow fiber film thread is sent into drying tunnel and is sintered 10~60 seconds in 100~130 DEG C to get enhancing polyethylene hollow fiber Film.
7. a kind of preparation method of enhanced polyethylene hollow fiber membrane according to claim 6, which is characterized in that described Winding layer number in step 3) is no more than 10 layers.
8. a kind of preparation method of enhanced polyethylene hollow fiber membrane according to claim 6, which is characterized in that described Organic fiber shell material in step 3) is aramid fiber, terylene, polyester, polyether-ether-ketone, PSA fiber, poly- paraphenylene terephthalamide to benzene two Amine, Visil fiber, polybenzimidazoles, polyphenylene sulfide or polyimides, 1-5.5 millimeters of sleeve outer, 0.5-4.5 millimeters of internal diameter.
CN201810517141.9A 2018-05-25 2018-05-25 A kind of enhanced polyethylene hollow fiber membrane and preparation method thereof Withdrawn CN110523298A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114950152A (en) * 2022-05-10 2022-08-30 苏州大学 Fiber tube reinforced hollow fiber membrane and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114950152A (en) * 2022-05-10 2022-08-30 苏州大学 Fiber tube reinforced hollow fiber membrane and preparation method thereof

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