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CN105797601A - Reinforced hollow fiber composite membrane and preparation method thereof - Google Patents

Reinforced hollow fiber composite membrane and preparation method thereof Download PDF

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Publication number
CN105797601A
CN105797601A CN201610176495.2A CN201610176495A CN105797601A CN 105797601 A CN105797601 A CN 105797601A CN 201610176495 A CN201610176495 A CN 201610176495A CN 105797601 A CN105797601 A CN 105797601A
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CN
China
Prior art keywords
hollow fiber
preparation
enhancement type
compound film
type hollow
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Pending
Application number
CN201610176495.2A
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Chinese (zh)
Inventor
陈亦力
丑树人
彭文娟
夏建中
林勇
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Beijing Originwater Membrane Technology Co Ltd
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Beijing Originwater Membrane Technology Co Ltd
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Priority to CN201610176495.2A priority Critical patent/CN105797601A/en
Publication of CN105797601A publication Critical patent/CN105797601A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06Organic material
    • B01D71/56Polyamides, e.g. polyester-amides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D67/00Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002Organic membrane manufacture
    • B01D67/0006Organic membrane manufacture by chemical reactions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/08Hollow fibre membranes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12Composite membranes; Ultra-thin membranes

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The invention discloses a reinforced hollow fiber composite membrane and a preparation method thereof.The preparation method is characterized in that hollow fiber ultrafiltration membrane yarn with an inner separation layer is prepared with a wet spinning process, filaments are adopted for knitting or crocheting on the outer surface of the hollow fiber membrane yarn, and a reinforced hollow fiber base membrane is obtained; a polyamide desalted layer is composited in an inner cavity of a fiber tube with an interfacial polymerization method, and the reinforced hollow fiber composite membrane is obtained.Higher mechanical strength of the membrane yarn is achieved with a netted support, and thus the reinforced hollow fiber composite membrane is suitable for the reverse osmosis and pressure-retarded osmosis processes performed at high pressure.

Description

A kind of enhancement type hollow fiber compound film and preparation method thereof
Technical field
The present invention relates to separation film composite material preparing technical field, particularly a kind of enhancement type hollow fiber compound film and preparation method thereof.
Background technology
The reverse osmosis membrane process such as Membrane seawater desalination, brackish water desalination that synthesizes of artificial semipermeable membrane has established technical foundation, and has promoted the development of Membrane Separation for Water Treatment.
Current reverse osmosis membrane mainly adopts the compound coiled reverse osmosis membrane of polyamide film and doughnut reverse osmosis membrane.
On the one hand, polyamide composite film has high flux, the feature of equipment with high desalinization.But, rolled film original paper complex manufacturing, the degree that becomes more meticulous height, and need substantial amounts of non-membrane material, for instance and dense water filter, pure water runner cloth, central canal etc., add the manufacturing cost of membrane component.
On the other hand, doughnut reverse osmosis membrane is with cellulose acetate or Triafol T for material of preparing, and this material is easily hydrolyzed under acid or alkali condition, and the toleration therefore acid, alkali cleaned is low;The characteristic of material itself also determines cellulose acetate reverse osmosis film needs higher operation pressure, namely higher energy expenditure.
For the problems referred to above, the present invention devises a kind of enhancement type hollow fiber compound film and preparation method thereof, doughnut polyamide film composite membrane obtained by the method can keep the feature of polyamide desalination layer high flux equipment with high desalinization on the one hand, can reduce the manufacturing cost of membrane component on the other hand.
But, due to the construction features of hollow-fibre membrane, the outer surface at doughnut passes through the mode synthesizing polyamides desalination layer of interfacial polymerization, and its uniformity is relatively difficult to ensure card;And it is higher in the feasibility of the inner surface synthesizing polyamides desalination layer of doughnut.In order to reduce the membrane area loss that inner surface complex form brings, hollow fiber film thread should select thin-wall construction, i.e. wall thickness/external diameter < 0.15, and this structure will greatly reduce the intensity of hollow fiber film thread.
Summary of the invention
The technical problem to be solved is to provide a kind of enhancement type hollow fiber compound film and preparation method thereof.Enhancement type hollow fiber film obtained by the method has higher mechanical strength, meets membrane process when high pressure operation, such as reverse osmosis and pressure retarded osmosis process..
A kind of enhancement type hollow fiber compound film, including outer layer network structure, intermediate porous transition zone, internal layer polyamide desalination layer.
Further, the cancellated thickness of described outer layer is 50-500 μm.
Further, the porosity of described intermediate porous transition zone is 50-85%, and thickness is 50-300 μm, and inner surface aperture is 5-50nm.
Further, described internal layer polyamide desalination layer pure water flux is 10-100L/ (m2H MPa), sodium chloride diffusibility is 0.05-5L/ (m2·h)。
Further, the tensile force of described enhancement type hollow fiber compound film is more than 10N, and burst pressure is more than 1MPa.
The preparation method that the invention also discloses a kind of enhancement type hollow fiber compound film, it is realized by the following step:
Preparation has interior stratum disjunctum hollow fiber film yarn, forms described intermediate porous transition zone;
At the outer surface of described described intermediate porous transition zone, filament fiber is adopted to carry out weaving or crocheting, it is thus achieved that enhancement mode doughnut basement membrane, outer layer network structure;
At described intermediate porous transition zone inner chamber, with interfacial polymerization composite polyamide desalination layer, form described internal layer polyamide desalination layer, and finally obtain enhancement type hollow fiber compound film.
Further, described preparation has the step of interior stratum disjunctum hollow fiber film yarn, adopts wet spinning technology to carry out, and its step is as follows:
Step 1), polymer, solvent, porogen are mixed according to following part by weight: polymer 10-30%, solvent 50-80%, porogen 10-20%, described mixture stirs 12-48h at 40-80 DEG C and obtains the casting solution of clear;
Step 2), by step 1) in the described casting solution that obtains extruded from spinning head by pressurized tank, enter and coagulation bath occur inversion of phases, it is thus achieved that there is the hollow fiber film thread of loose structure.
Further, described polymer adopts the arbitrary proportion mixture of one or more in polysulfones, polyether sulfone, Kynoar, polyimides, Polyetherimide, polyacrylonitrile.
Further, described solvent adopts the arbitrary proportion mixture of one or more in dimethylformamide, dimethyl acetylamide, dimethyl sulfoxide, N, N-dimethyl pyrrolidone.
Further, described porogen adopts the arbitrary proportion mixture of one or more in lithium chloride, lithium perchlorate, ethanol, ethylene glycol, propylene glycol, glycerol, Polyethylene Glycol, polyvinylpyrrolidone.
Further, the central canal external diameter 0.5-1.5mm of spinning head, spinning head spray orifice internal diameter is 1.0-3.0mm.
Further, described coagulation bath adopts the one of deionized water and described solvent or its arbitrary proportion mixture as medium.
Further, described establishment or crocheting, complete according to the following steps: by the hollow fiber film thread collected by braider or cloche, filament fiber is compounded in the outer surface of hollow fiber film thread, forms enhancement mode doughnut basement membrane;Selected braiding number of spindles is 4-32 ingot, and bipatch is 10-25mm;Selected crocheting pin number is 3-12 pin, and crocheting density is 5-20 order.
Further, described filament fiber adopts nylon, polypropylene, polyethylene.
Further, described interfacial polymerization, have the following step to realize:
At described enhancement mode doughnut basement membrane inner surface, successively the contact aqueous phase solution containing polyamine, compression air, containing the organic phase solution of polynary acyl chlorides, deionized water.
Further, in described aqueous phase solution, in mass fraction, polyamine is 0.5-5%, triethylamine is 0-5%, camphorsulfonic acid 0-5%.
Further, described polyamine includes m-diaminobenzene., p-phenylenediamine, ethylenediamine, piperazine.
Further, described compression air-operated pressure is 0.01-1MPa.
Further, in described organic phase solution, solvent is at least one in pentane, normal hexane, hexamethylene, ethyl cyclohexane;Polynary acyl chlorides mass fraction is 0.05-0.5%.
Further, described polynary acyl chlorides is at least one in pyromellitic trimethylsilyl chloride, m-phthaloyl chloride.
The useful fruit of the present invention is in that: take the mode of filament fiber braiding or crocheting to promote the intensity of interior layer composite hollow-fibre membrane, to adapt to membrane process when high pressure operation, such as reverse osmosis and pressure retarded osmosis process.First pass through wet spinning technology and prepare doughnut basement membrane.Specifically, polymeric material it is dissolved in selected solvent and adds organic or inorganic porogen and be configured to casting solution.Described casting solution is extruded through spinneret, solidify to form the doughnut basement membrane of new life after entering coagulation bath generation inversion of phases.In order to strengthen the mechanical strength that doughnut is, the outer surface at described doughnut basement membrane forms network-like reinforced structure by the mode of braiding or crocheting, forms strengthening doughnut basement membrane.Owing to establishment or crocheting adopt long fibre, described network-like reinforced structure has higher tensile strength, provides mechanical support for described doughnut basement membrane, breaks resisting the deformation under high pressure operation.At the inner surface of described strengthening doughnut basement membrane, form polyamide desalination layer by interfacial polymerization, it is thus achieved that there is the hollow fiber composite membrane of desalination function.Specifically, with the inner surface of the infiltration strengthened doughnut basement membrane of the aqueous phase solution containing polyamine, after removing unnecessary aqueous phase solution, contact the inner surface of doughnut with organic phase solution, interfacial polymerization occurs to go out at the interface of aqueous phase solution and organic phase solution, forms polyamide functional layer.
Accompanying drawing explanation
Fig. 1 is the structural representation of enhancement type hollow fiber compound film.
Detailed description of the invention
Below in conjunction with drawings and Examples, the specific embodiment of the present invention being further described, following example are only for clearly illustrating technical scheme, and can not limit the scope of the invention with this.
The concrete technical scheme of the present invention is as follows:
As it is shown in figure 1, a kind of enhancement type hollow fiber compound film, including outer layer network structure 1, intermediate porous transition zone 2, internal layer polyamide desalination layer 3;The thickness of described outer layer network structure 1 is 50-500 μm;The porosity of described intermediate porous transition zone 2 is 50-85%, and thickness is 50-300 μm, and inner surface aperture is 5-50nm;Described internal layer polyamide desalination layer 3 pure water flux is 10-100L/ (m2H MPa), sodium chloride diffusibility is 0.05-5L/ (m2·h);The tensile force of described enhancement type hollow fiber compound film is more than 10N, and burst pressure is more than 1MPa.
The preparation method that the invention also discloses a kind of enhancement type hollow fiber compound film, it is realized by the following step:
First, adopt wet spinning technology preparation to have interior stratum disjunctum hollow fiber film yarn, form described intermediate porous transition zone;Described wet spinning technology, comprises the steps:
Step 1), polymer, solvent, porogen are mixed according to following part by weight: polymer 10-30%, solvent 50-80%, porogen 10-20%, described mixture stirs 12-48h at 40-80 DEG C and obtains the casting solution of clear;Described polymer adopts the arbitrary proportion mixture of one or more in polysulfones, polyether sulfone, Kynoar, polyimides, Polyetherimide, polyacrylonitrile;Described solvent adopts the arbitrary proportion mixture of one or more in dimethylformamide, dimethyl acetylamide, dimethyl sulfoxide, N, N-dimethyl pyrrolidone;Described porogen adopts the arbitrary proportion mixture of one or more in lithium chloride, lithium perchlorate, ethanol, ethylene glycol, propylene glycol, glycerol, Polyethylene Glycol, polyvinylpyrrolidone;
Step 2), by step 1) in the described casting solution that obtains extruded from spinning head by pressurized tank, enter and coagulation bath occur inversion of phases, it is thus achieved that there is the hollow fiber film thread of loose structure;The central canal external diameter 0.5-1.5mm of spinning head, spinning head spray orifice internal diameter is 1.0-3.0mm;The one of described coagulation bath employing deionized water and described solvent or its arbitrary proportion mixture are as medium.
Secondly, at the outer surface of described described intermediate porous transition zone, adopt filament fiber to carry out weaving or crocheting, it is thus achieved that enhancement mode doughnut basement membrane, outer layer network structure;Described establishment or crocheting, complete according to the following steps: the hollow fiber film thread collected is passed through braider or cloche, filament fiber is compounded in the outer surface of hollow fiber film thread, form enhancement mode doughnut basement membrane;Selected braiding number of spindles is 4-32 ingot, and bipatch is 10-25mm;Selected crocheting pin number is 3-12 pin, and crocheting density is 5-20 order;
At described intermediate porous transition zone inner chamber, with interfacial polymerization composite polyamide desalination layer, form described internal layer polyamide desalination layer, and finally obtain enhancement type hollow fiber compound film.Described filament fiber adopts nylon, polypropylene, polyethylene.
Described interfacial polymerization, has the following step to realize:
At described enhancement mode doughnut basement membrane inner surface, successively the contact aqueous phase solution containing polyamine, compression air, containing the organic phase solution of polynary acyl chlorides, deionized water.
In described aqueous phase solution, in mass fraction, polyamine is 0.5-5%, triethylamine is 0-5%, camphorsulfonic acid 0-5%.
Described polyamine includes m-diaminobenzene., p-phenylenediamine, ethylenediamine, piperazine.
Described compression air-operated pressure is 0.01-1MPa.
In described organic phase solution, solvent is at least one in pentane, normal hexane, hexamethylene, ethyl cyclohexane;Polynary acyl chlorides mass fraction is 0.05-0.5%.
Described polynary acyl chlorides is at least one in pyromellitic trimethylsilyl chloride, m-phthaloyl chloride.
The above is only the preferred embodiments of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from the technology of the present invention principle; can also making some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.

Claims (10)

1. an enhancement type hollow fiber compound film, it is characterised in that include outer layer network structure (1), intermediate porous transition zone (2), internal layer polyamide desalination layer (3).
2. a kind of enhancement type hollow fiber compound film as claimed in claim 1, it is characterized in that, the thickness of described outer layer network structure (1) is 50-500 μm, the porosity of described intermediate porous transition zone (2) is 50-85%, thickness is 50-300 μm, and inner surface aperture is 5-50nm.
3. a kind of enhancement type hollow fiber compound film as claimed in claim 1, it is characterised in that described internal layer polyamide desalination layer (3) pure water flux is 10-100L/ (m2H MPa), sodium chloride diffusibility is 0.05-5L/ (m2·h)。
4. the preparation method of an enhancement type hollow fiber compound film, it is characterised in that it is realized by the following step:
Preparation has interior stratum disjunctum hollow fiber film yarn, forms intermediate porous transition zone;
At the outer surface of described intermediate porous transition zone, adopt filament fiber to carry out weaving or crocheting, it is thus achieved that enhancement mode doughnut basement membrane, form outer layer network structure;
At described intermediate porous transition zone inner chamber, polymerization forms described internal layer polyamide desalination layer, to obtain enhancement type hollow fiber compound film.
5. the preparation method of enhancement type hollow fiber compound film as claimed in claim 4, it is characterised in that described preparation has the step of interior stratum disjunctum hollow fiber film yarn, adopts wet spinning technology to carry out, and its step is as follows:
Step 1), polymer, solvent, porogen are mixed according to following part by weight: polymer 10-30%, solvent 50-80%, porogen 10-20%, described mixture stirs acquisition casting solution at 40-80 DEG C;
Step 2), by step 1) in the described casting solution that obtains extruded from spinning head by pressurized tank, enter and coagulation bath occur inversion of phases, it is thus achieved that there is the hollow fiber film thread of loose structure.
6. the preparation method of enhancement type hollow fiber compound film as claimed in claim 4, it is characterized in that, described employing filament fiber carries out weaving or crocheting, obtain enhancement mode doughnut basement membrane, form outer layer network structure, farther include establishment or crocheting, complete according to the following steps: the hollow fiber film thread collected is passed through braider or cloche, filament fiber is compounded in the outer surface of hollow fiber film thread, forms enhancement mode doughnut basement membrane;Selected braiding number of spindles is 4-32 ingot, and bipatch is 10-25mm;Selected crocheting pin number is 3-12 pin, and crocheting density is 5-20 order.
7. the preparation method of enhancement type hollow fiber compound film as claimed in claim 4, it is characterised in that described filament fiber adopts in nylon, polypropylene, polyethylene at least one.
8. the preparation method of enhancement type hollow fiber compound film as claimed in claim 4, it is characterized in that, described interfacial polymerization, realized by following steps: at described enhancement mode doughnut basement membrane inner surface, successively the contact aqueous phase solution containing polyamine, compression air, containing the organic phase solution of polynary acyl chlorides, deionized water.
9. the preparation method of enhancement type hollow fiber compound film as claimed in claim 8, it is characterised in that in described aqueous phase solution, in mass fraction, polyamine is 0.5-5%, triethylamine is 0-5%, camphorsulfonic acid 0-5%;Described polyamine includes in m-diaminobenzene., p-phenylenediamine, ethylenediamine, piperazine at least one;Compression air-operated pressure is 0.01-1MPa.
10. the preparation method of a kind of enhancement type hollow fiber compound film as claimed in claim 8, it is characterised in that in described organic phase solution, solvent is at least one in pentane, normal hexane, hexamethylene, ethyl cyclohexane;Polynary acyl chlorides mass fraction is 0.05-0.5%;Described polynary acyl chlorides is at least one in pyromellitic trimethylsilyl chloride, m-phthaloyl chloride.
CN201610176495.2A 2016-03-25 2016-03-25 Reinforced hollow fiber composite membrane and preparation method thereof Pending CN105797601A (en)

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Cited By (7)

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CN106621849A (en) * 2016-12-21 2017-05-10 天津膜天膜科技股份有限公司 Polyamide hollow fiber nanofiltration membrane and preparation method thereof
WO2018018501A1 (en) * 2016-07-28 2018-02-01 Honeywell International Inc. Reverse osmosis membrane and method of processing the same
WO2019108136A1 (en) * 2017-11-30 2019-06-06 National University Of Singapore A thin film composite hollow fibre membrane
CN112007519A (en) * 2020-08-17 2020-12-01 杭州科百特科技有限公司 Oxygenation membrane, preparation method thereof and oxygenation assembly
CN112337317A (en) * 2019-08-07 2021-02-09 北京新源国能科技集团股份有限公司 Enhanced hollow fiber composite nanofiltration membrane and preparation method thereof
CN112774465A (en) * 2020-12-25 2021-05-11 湖南澳维环保科技有限公司 Polyamide composite membrane, preparation method thereof and membrane element
CN113490542A (en) * 2019-02-28 2021-10-08 株式会社可乐丽 Composite hollow fiber membrane and method for producing composite hollow fiber membrane

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CN202638295U (en) * 2012-06-29 2013-01-02 北京碧水源膜科技有限公司 External support reinforced hollow fiber nanofiltration membrane
CN103111195A (en) * 2013-03-13 2013-05-22 株洲时代新材料科技股份有限公司 High-temperature resistance polyamide composite membrane and preparation method thereof
CN103638832A (en) * 2013-11-14 2014-03-19 株洲时代新材料科技股份有限公司 Polyamide composite membrane and production method thereof

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Publication number Priority date Publication date Assignee Title
CN1380130A (en) * 2002-02-07 2002-11-20 尉福生 Preparation method of hollow fibre supermicro filtration membrane
CN202638295U (en) * 2012-06-29 2013-01-02 北京碧水源膜科技有限公司 External support reinforced hollow fiber nanofiltration membrane
CN103111195A (en) * 2013-03-13 2013-05-22 株洲时代新材料科技股份有限公司 High-temperature resistance polyamide composite membrane and preparation method thereof
CN103638832A (en) * 2013-11-14 2014-03-19 株洲时代新材料科技股份有限公司 Polyamide composite membrane and production method thereof

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018018501A1 (en) * 2016-07-28 2018-02-01 Honeywell International Inc. Reverse osmosis membrane and method of processing the same
CN109414659A (en) * 2016-07-28 2019-03-01 霍尼韦尔国际公司 Reverse osmosis membrane and its processing method
EP3490698A4 (en) * 2016-07-28 2020-03-25 Honeywell International Inc. Reverse osmosis membrane and method of processing the same
CN106621849A (en) * 2016-12-21 2017-05-10 天津膜天膜科技股份有限公司 Polyamide hollow fiber nanofiltration membrane and preparation method thereof
WO2019108136A1 (en) * 2017-11-30 2019-06-06 National University Of Singapore A thin film composite hollow fibre membrane
CN111405939A (en) * 2017-11-30 2020-07-10 新加坡国立大学 Thin film composite hollow fiber membrane
US11465100B2 (en) 2017-11-30 2022-10-11 National University Of Singapore Thin film composite hollow fibre membrane
CN113490542A (en) * 2019-02-28 2021-10-08 株式会社可乐丽 Composite hollow fiber membrane and method for producing composite hollow fiber membrane
CN112337317A (en) * 2019-08-07 2021-02-09 北京新源国能科技集团股份有限公司 Enhanced hollow fiber composite nanofiltration membrane and preparation method thereof
CN112007519A (en) * 2020-08-17 2020-12-01 杭州科百特科技有限公司 Oxygenation membrane, preparation method thereof and oxygenation assembly
CN112007519B (en) * 2020-08-17 2023-05-02 杭州科百特科技有限公司 Oxygenation membrane, preparation method thereof and oxygenation assembly
CN112774465A (en) * 2020-12-25 2021-05-11 湖南澳维环保科技有限公司 Polyamide composite membrane, preparation method thereof and membrane element
CN112774465B (en) * 2020-12-25 2022-04-15 湖南澳维科技股份有限公司 Polyamide composite membrane, preparation method thereof and membrane element

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