CN106582297A - Preparation method of high-performance nanofiltration membrane for water purifier - Google Patents

Preparation method of high-performance nanofiltration membrane for water purifier Download PDF

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Publication number
CN106582297A
CN106582297A CN201611106613.9A CN201611106613A CN106582297A CN 106582297 A CN106582297 A CN 106582297A CN 201611106613 A CN201611106613 A CN 201611106613A CN 106582297 A CN106582297 A CN 106582297A
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Prior art keywords
membrane
preparation
performance
layer
water purifier
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CN201611106613.9A
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Inventor
翁华明
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Suzhou Rich Industrial Equipment Co Ltd
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Suzhou Rich Industrial Equipment Co Ltd
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Priority to CN201611106613.9A priority Critical patent/CN106582297A/en
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    • 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
    • B01D71/08—Polysaccharides
    • B01D71/12—Cellulose derivatives
    • B01D71/14—Esters of organic acids
    • 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
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • 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
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • B01D69/122—Separate manufacturing of ultra-thin 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
    • B01D71/08—Polysaccharides
    • B01D71/12—Cellulose derivatives
    • B01D71/14—Esters of organic acids
    • B01D71/16—Cellulose acetate
    • 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
    • B01D71/26—Polyalkenes
    • 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
    • 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
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
    • B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
    • 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
    • B01D71/56—Polyamides, e.g. polyester-amides
    • 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
    • B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
    • B01D71/62—Polycondensates having nitrogen-containing heterocyclic rings in the main chain
    • B01D71/64—Polyimides; Polyamide-imides; Polyester-imides; Polyamide acids or similar polyimide precursors
    • 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
    • B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
    • B01D71/68—Polysulfones; Polyethersulfones
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/36—Hydrophilic membranes

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

Abstract

The invention relates to a preparation method of a high-performance nanofiltration membrane for a water purifier. The preparation method includes the following steps that 1, a steel wire net is made into a cuboid shape, and a supporting layer is made; 2, the surface of the made supporting layer is covered with a porous carrier layer; 3, the surface of the porous carrier layer is covered with a nanofiltration membrane layer; 4, the outer surface of the nanofiltration membrane layer is coated with a protective layer, and the high-performance nanofiltration membrane for the water purifier is prepared. According to the preparation method of the high-performance nanofiltration membrane for the water purifier, a good interception effect is achieved for ions through intervals between graphene oxide layers, hydrophilia can be improved through oxygen-containing functional groups on the surfaces, the membrane has good permeability and retention performance, and filtering of the nanofiltration membrane layer is more efficient.

Description

A kind of water purifier preparation method of high-performance NF membrane
Technical field
The present invention relates to a kind of preparation method of water purifier with high-performance NF membrane, belongs to filter plant technical field.
Background technology
NF membrane：In more than 1nm, general 1-2nm is to allow solvent molecule or some low molecular weight solutes or low price in aperture A kind of functional semipermeable membrane of ion permeable.It is a kind of special and up-and-coming seperation film kind, and it is because retaining The size of material is about nanometer and gains the name, and it is about 150-500 or so that it retains the molecular weight of Organic substance, retains dissolubility salt Ability be between 2-98%, high-valence anion saline solution to be less than to the desalination of monovalent anion saline solution.It is used to remove ground The Organic substance and colourity of table water, removes underground hardness of water, and part removes dissolubility salt, in concentrated fruit juice and separation medicine Utility etc..
NF membrane is the key of nanofiltration process, and requirement of the nanofiltration to membrane material is：With good film property, thermally-stabilised Property, chemical stability, high mechanical strength, acid and alkali-resistance and microbial attack, chlorine-resistant and other oxidizing substances, have high water flux and High salt rejection rate, anticol body and suspended solid pollutant, low price and the NF membrane for adopting mostly are aromatic series and polyacids hydrogen species are compound NF membrane.Composite membrane is anisotropic membrane, is made up of two-part structure：A part is passive perforated membrane, and its mechanism is Sieving actoion;Another part has been the dense film of the layer of centrifugation, and its separating mechanism can be entered with dissolve-diffusion model Row is explained.For composite membrane, the optimization of material and structure can be respectively carried out to the epidermal area of a centrifugation and supporting layer, can The composite membrane of excellent.The form of membrane module has doughnut, rolling, plate and frame and tubular type etc..Wherein, doughnut It is high with the packed density of rolled membrane module, low cost, hydrodynamic conditions are good in component;But the manufacture skill of both membrane modules Art has high demands, and sealing is difficult, and contamination resistance is poor in use, high to feed liquid pre-processing requirements.And plate and frame and tubular membrane component Although easy to clean, anti-pollution, the packed density of film is low, cost is high.Therefore, it is in nanofiltration system to use hollow fiber form more Or rolled membrane module.
The content of the invention
The technical problem to be solved in the present invention is, not enough for prior art, proposes that one kind can be applied in combination and improved Filter the preparation method of the water purifier with high-performance NF membrane of performance.
The present invention is that the technical scheme for solving above-mentioned technical problem proposition is：A kind of water purifier system of high-performance NF membrane Preparation Method, comprises the following steps：
(i). rectangular-shape is made as using steel wire, supporting layer is obtained；
(ii). cover porous carrier layer in obtained support layer surface；
(iii). nanofiltration film layer is covered in porous carrier layer surface, the preparation method of the nanofiltration film layer is comprised the following steps：
A. it is that 98% concentrated sulphuric acid adds into expansible graphite raw material by mass fraction in 0 DEG C of ice-water bath, is slowly added Gao Meng Sour potassium, stirs, and is placed in water bath with thermostatic control and is heated to 45～50 DEG C, keeps 0.5-2h；
B. deionized water is slowly added dropwise in resulting solution in step A to produce to reaction system bubble-free, is heated up in water bath with thermostatic control To 95-100 DEG C, 25-30 minutes are stirred, hydrogen peroxide solution to the solution that mass fraction is 25% is added after natural cooling and is changed into bright The suspension of yellow；
C. step B gained suspension is filtered into obtain brown color colloid, Jing pickling and deionized water wash are dried after super to neutrality Ultrasonic disperse and centrifugally operated in pure water, supernatant is placed in 65～75 DEG C of drying bakers and dries to obtain graphene oxide powder；
D. gained graphene oxide powder is placed in ultrasonic disperse 1-5h in polar solvent in step C, and supernatant is removed after centrifugation, obtains To graphene oxide solution；
E. with polymer ultrafiltration membrane as basement membrane, graphene oxide solution is filtered using basement membrane, under 0.05-0.5MPa static pressures Constantly promote graphene oxide solution to make solvent molecule pass through ultrafilter membrane, obtain the nanofiltration film layer of moistening；
F. the product for covering the nanofiltration film layer of moistening is placed in vacuum drying oven and is dried, final nanofiltration film layer is obtained；
(iv). it is armor coated in nanofiltration film layer outer surface, the protective layer adopt concentration for 11-15% PVA aqueous solutions with receive Filter membranous layer reaction is placed in being dried in vacuum drying oven, and water purifier high-performance NF membrane is obtained.
The improvement of above-mentioned technical proposal is：Water purifier is with the step of the preparation method of high-performance NF membrane (iii) in middle operation D Polar solvent is water or alcohols.
The improvement of above-mentioned technical proposal is：Water purifier with the step of the preparation method of high-performance NF membrane (iii) in macromolecule Ultrafiltration membrane material be polyether sulfone, polyacrylonitrile, polypropylene, polyethylene, Kynoar, cellulose acetate, cellulose diacetate, Triafol T, cellulose propionate, cellulose butyrate, cellulose acetate propionate, two cellulose butyrates, three cellulose butyrates, Vinegar polyacrylonitrile, Polyurethane, polrvinyl chloride, polyether-ether-ketone, sulfonated polyether-ether-ketone, sulfonated polyimide, sulfonated polyether sulfone, sulfonation Any one or more in polysulfones, polybenzimidazoles, polycaprolactam or poly- furan alcohol.
The present invention is using the beneficial effect of above-mentioned technical proposal：
（1）The oxygen-containing functional group that graphene oxide interlamellar spacing also has good crown_interception, its surface to ion can also increase parent Aqueouss, and then make film possess good permeability and rejection so that the filtration of nanofiltration film layer is more efficient；
（2）There are a large amount of free carboxyls and hydroxyl in the film surface of nanofiltration film layer, with high-hydrophilic, high-throughout feature, while Film surface bear electricity, can effectively improve salt-stopping rate, so as to significantly improve the flux and desalting effect of NF membrane, substantially increase Strainability, with good heavy industrialization application prospect；
（3）Because the outer surface of nanofiltration film layer is also covered with protective layer, effectively prevent from causing nanofiltration because outside debris etc. collide with The breakage of film layer, so as to cause situations such as filtering not thorough, filters the efficiency of work.
Specific embodiment
Embodiment one
The preparation method of the water purifier high-performance NF membrane of the present embodiment is comprised the following steps：
(i). rectangular-shape is made as using steel wire, supporting layer is obtained；
(ii). cover porous carrier layer in obtained support layer surface；
(iii). nanofiltration film layer is covered in porous carrier layer surface, the preparation method of the nanofiltration film layer is comprised the following steps：
A. it is that 98% concentrated sulphuric acid adds into expansible graphite raw material by mass fraction in 0 DEG C of ice-water bath, is slowly added Gao Meng Sour potassium, stirs, and is placed in water bath with thermostatic control and is heated to 45～50 DEG C, keeps 0.5-2h；
B. deionized water is slowly added dropwise in resulting solution in step A to produce to reaction system bubble-free, is heated up in water bath with thermostatic control To 95-100 DEG C, 25-30 minutes are stirred, hydrogen peroxide solution to the solution that mass fraction is 25% is added after natural cooling and is changed into bright The suspension of yellow；
C. step B gained suspension is filtered into obtain brown color colloid, Jing pickling and deionized water wash are dried after super to neutrality Ultrasonic disperse and centrifugally operated in pure water, supernatant is placed in 65～75 DEG C of drying bakers and dries to obtain graphene oxide powder；
D. gained graphene oxide powder is placed in ultrasonic disperse 1-5h in polar solvent in step C, and supernatant is removed after centrifugation, obtains To graphene oxide solution；
E. with polymer ultrafiltration membrane as basement membrane, graphene oxide solution is filtered using basement membrane, under 0.05-0.5MPa static pressures Constantly promote graphene oxide solution to make solvent molecule pass through ultrafilter membrane, obtain the nanofiltration film layer of moistening；
F. the product for covering the nanofiltration film layer of moistening is placed in vacuum drying oven and is dried, final nanofiltration film layer is obtained；
(iv). it is armor coated in nanofiltration film layer outer surface, the protective layer adopt concentration for 11-15% PVA aqueous solutions with receive Filter membranous layer reaction is placed in being dried in vacuum drying oven, and water purifier high-performance NF membrane is obtained.
In the preparation method：Water purifier (iii) polar solvent in middle operation D the step of the preparation method of high-performance NF membrane For water or alcohols.
In the preparation method：Water purifier with the step of the preparation method of high-performance NF membrane (iii) in polymer ultrafiltration membrane material Expect for polyether sulfone, polyacrylonitrile, polypropylene, polyethylene, Kynoar, cellulose acetate, cellulose diacetate, three acetic acid fibre Dimension element, cellulose propionate, cellulose butyrate, cellulose acetate propionate, two cellulose butyrates, three cellulose butyrates, vinegar polypropylene It is nitrile, Polyurethane, polrvinyl chloride, polyether-ether-ketone, sulfonated polyether-ether-ketone, sulfonated polyimide, sulfonated polyether sulfone, SPSF, poly- Any one or more in benzimidazole, polycaprolactam or poly- furan alcohol.
The present invention is not limited to above-described embodiment.The technical scheme that all employing equivalents are formed, all falling within the present invention will The protection domain asked.

Claims (4)

1. a kind of water purifier preparation method of high-performance NF membrane, it is characterised in that：Comprise the following steps：
(i). rectangular-shape is made as using steel wire, supporting layer is obtained；
(ii). cover porous carrier layer in obtained support layer surface；
(iii). nanofiltration film layer is covered in porous carrier layer surface, the preparation method of the nanofiltration film layer is comprised the following steps：
A. it is that 98% concentrated sulphuric acid adds into expansible graphite raw material by mass fraction in 0 DEG C of ice-water bath, is slowly added Gao Meng Sour potassium, stirs, and is placed in water bath with thermostatic control and is heated to 45～50 DEG C, keeps 0.5-2h；
B. deionized water is slowly added dropwise in resulting solution in step A to produce to reaction system bubble-free, is heated up in water bath with thermostatic control To 95-100 DEG C, 25-30 minutes are stirred, hydrogen peroxide solution to the solution that mass fraction is 25% is added after natural cooling and is changed into bright The suspension of yellow；
C. step B gained suspension is filtered into obtain brown color colloid, Jing pickling and deionized water wash are dried after super to neutrality Ultrasonic disperse and centrifugally operated in pure water, supernatant is placed in 65～75 DEG C of drying bakers and dries to obtain graphene oxide powder；
D. gained graphene oxide powder is placed in ultrasonic disperse 1-5h in polar solvent in step C, and supernatant is removed after centrifugation, obtains To graphene oxide solution；
E. with polymer ultrafiltration membrane as basement membrane, graphene oxide solution is filtered using basement membrane, under 0.05-0.5MPa static pressures Constantly promote graphene oxide solution to make solvent molecule pass through ultrafilter membrane, obtain the nanofiltration film layer of moistening；
F. the product for covering the nanofiltration film layer of moistening is placed in vacuum drying oven and is dried, final nanofiltration film layer is obtained；
(iv). it is armor coated in nanofiltration film layer outer surface, the protective layer adopt concentration for 11-15% PVA aqueous solutions with receive Filter membranous layer reaction is placed in being dried in vacuum drying oven, and water purifier high-performance NF membrane is obtained.
2. the water purifier according to claim 1 preparation method of high-performance NF membrane, it is characterised in that：The porous is carried Body layer is made up of one or more in textile fabric, adhesive-bonded fabric and microporous membrane.
3. the water purifier according to claim 2 preparation method of high-performance NF membrane, it is characterised in that：The water purifier With the step of the preparation method of high-performance NF membrane, (iii) polar solvent is water or alcohols in middle operation D.
4. the water purifier according to claim 3 preparation method of high-performance NF membrane, it is characterised in that：The water purifier With the step of the preparation method of high-performance NF membrane (iii) described in polymer ultrafiltration membrane material be polyether sulfone, polyacrylonitrile, poly- Propylene, polyethylene, Kynoar, cellulose acetate, cellulose diacetate, Triafol T, cellulose propionate, butanoic acid are fine Dimension element, cellulose acetate propionate, two cellulose butyrates, three cellulose butyrates, vinegar polyacrylonitrile, Polyurethane, polrvinyl chloride, polyethers Ether ketone, sulfonated polyether-ether-ketone, sulfonated polyimide, sulfonated polyether sulfone, SPSF, polybenzimidazoles, polycaprolactam or poly- Any one or more in furan alcohol.
CN201611106613.9A 2016-12-06 2016-12-06 Preparation method of high-performance nanofiltration membrane for water purifier Pending CN106582297A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111715078A (en) * 2019-03-20 2020-09-29 暨南大学 Sandwich graphene oxide hollow fiber membrane with fixed interlamellar spacing and preparation method and application thereof
CN112295418A (en) * 2019-07-30 2021-02-02 上海恩捷新材料科技有限公司 Polyethylene-based composite graphene oxide nanofiltration membrane and preparation method thereof
CN115245757A (en) * 2021-04-28 2022-10-28 中国石油化工股份有限公司 Composite nanofiltration membrane and preparation method and application thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102989330A (en) * 2012-12-20 2013-03-27 浙江工商大学 Hybrid graphene/aromatic polyamide reverse osmosis membrane and preparation method thereof
CN103706264A (en) * 2014-01-14 2014-04-09 中国海洋大学 Layer-by-layer self-assembling oxidized graphene nano-filtration membrane and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102989330A (en) * 2012-12-20 2013-03-27 浙江工商大学 Hybrid graphene/aromatic polyamide reverse osmosis membrane and preparation method thereof
CN103706264A (en) * 2014-01-14 2014-04-09 中国海洋大学 Layer-by-layer self-assembling oxidized graphene nano-filtration membrane and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
于洪全: "《功能材料》", 30 June 2014, 北京交通大学出版社 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111715078A (en) * 2019-03-20 2020-09-29 暨南大学 Sandwich graphene oxide hollow fiber membrane with fixed interlamellar spacing and preparation method and application thereof
CN112295418A (en) * 2019-07-30 2021-02-02 上海恩捷新材料科技有限公司 Polyethylene-based composite graphene oxide nanofiltration membrane and preparation method thereof
CN115245757A (en) * 2021-04-28 2022-10-28 中国石油化工股份有限公司 Composite nanofiltration membrane and preparation method and application thereof
CN115245757B (en) * 2021-04-28 2023-07-21 中国石油化工股份有限公司 Composite nanofiltration membrane and preparation method and application thereof

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Application publication date: 20170426