CN107158971A - A kind of preparation method of composite nanometer filtering film - Google Patents

A kind of preparation method of composite nanometer filtering film Download PDF

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Publication number
CN107158971A
CN107158971A CN201710431105.6A CN201710431105A CN107158971A CN 107158971 A CN107158971 A CN 107158971A CN 201710431105 A CN201710431105 A CN 201710431105A CN 107158971 A CN107158971 A CN 107158971A
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CN
China
Prior art keywords
film
composite nanometer
nanometer filtering
filtering film
polyvinyl chloride
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710431105.6A
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Chinese (zh)
Inventor
王宁
陈瑶
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Zhejiang Ruisheng Environmental Protection Technology Co Ltd
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Zhejiang Ruisheng Environmental Protection Technology Co Ltd
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Priority to CN201710431105.6A priority Critical patent/CN107158971A/en
Publication of CN107158971A publication Critical patent/CN107158971A/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
    • B01D71/58Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
    • 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
    • B01D67/0009Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
    • 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

Abstract

The invention discloses a kind of preparation method of composite nanometer filtering film, the composite nanometer filtering film includes non-woven fabrics basement membrane, positioned at the epilamellar chliorinated polyvinyl chloride supporting layer of non-woven fabrics and the aromatic polyamides separating layer positioned at the chliorinated polyvinyl chloride supporting layer;The preparation method of the composite nanometer filtering film comprises the following steps:Prepare the non-woven fabrics basement membrane for being coated with chliorinated polyvinyl chloride supporting layer;Prepare the aromatic polyamides separating layer positioned at the chliorinated polyvinyl chloride supporting layer.Using above-mentioned technical proposal, the preparation method of composite nanometer filtering film of the invention, formula is simple, and technological operation is convenient, it is easy to industrialized production.Using the technology of the present invention, obtained composite nanometer filtering film has preferable chemical stability and resistance tocrocking, is more than 97% to magnesium sulfate rejection rate, is more than 85% to sodium chloride rejection.

Description

A kind of preparation method of composite nanometer filtering film
Technical field
The present invention relates to a kind of preparation method of composite nanometer filtering film, belong to water filtration technology field.
Background technology
It is contaminated now with substantial amounts of water so that the production and living of people, which are received on many influences, the earth, major part Area be that but seawater cannot be used by desalination.But the shortage of water resource and pollution cause the sharp again of water With long time is needed, only water can just be used by filtering with technical finesse, but existing technology causes processing The use that water people afterwards dare not trust, and it is contaminated after water in contain substantial amounts of harmful substance, endanger the health of people. Simultaneously for the use of city tap-water, although there is clear and definite drinking water standard in country, but increasing people still selects Running water carries out filtration treatment using preceding, to reduce infringement of the water pollution to health.Water circulation application is also water-saving one Item important measures, and it is necessary that using filtering technique in water cycle process.Generally for the filter element bag of water filtration Include coarse filtration filter core, membrane cartridge, absorption filter element etc., wherein coarse filtration filter core refers to the filter core for possessing coarse filtration function, including with quartz sand, The filter core of the filtrates such as anthracite, natural manganese sand, ceramics, PP cottons, membrane cartridge refers to the filter core constituted using membrane component as core, including Micro-filtration(MF)Filter core, ultrafiltration(UF)Filter core, nanofiltration(NF)Filter core, counter-infiltration(RO)Filter core etc., absorption filter element refers to possess absorption The filter core of function, including with granular activated carbon(GAC), active carbon stick(SAC), NACF(FAC), polymeric adsorbent, ceramics Particle etc. is the filter core of filtrate.
At present, Nanofiltration-membrane technique is state-of-the-art separation and filtering technique in the world, and due to extensive market, countries in the world are confused Confused organizational strength is put into the exploitation of Nanofiltration-membrane technique.The kind of NF membrane is continuously increased, and performance is improved constantly.It, which develops, becomes Gesture is to develop heat-resisting, acid and alkali-resistance, resistance to oxidation, resistance to free chlorine, high water flux, high rejection, resistant to pollution high-performance NF membrane.Film Material has cellulose acetate, aromatic polyamides, sulfonated polyether sulfone etc..At the nanofiltration at home and abroad water of successful operation Manage from the point of view of case history, its separating property is good, and stable effluent quality is reliable, and energy consumption is low, passed through with preferable technology Ji property.Although the domestic development of NF membrane in recent years is very fast, successively researched and developed a variety of NF membranes, it is most of all also in Laboratory research development phase, not yet commercialization.The chemical stability and resistance tocrocking of film are all poor.Wherein key also resides in film The selection of material and preparation technology are immature.
The content of the invention
Therefore, it is an object of the invention to provide a kind of preparation method of composite nanometer filtering film, so as to reach that NF membrane is easy to Industrialized production, performance is stable, the strong beneficial effect of antifouling property.
To achieve these goals, a kind of preparation method of composite nanometer filtering film of the invention, the composite nanometer filtering film includes nothing Spin cloth basement membrane, positioned at the epilamellar chliorinated polyvinyl chloride supporting layer of non-woven fabrics and positioned at the chliorinated polyvinyl chloride supporting layer Aromatic polyamides separating layer;The preparation method of the composite nanometer filtering film comprises the following steps:
1)It is 12 that chliorinated polyvinyl chloride, dimethylformamide and calcium chloride are pressed into quality parts ratio:18:6 ratio is weighed After mix;
2)The mixed liquor of step 1 is stirred and 70-80 °C is gradually heating to, makes chliorinated polyvinyl chloride, dimethylformamide and chlorine Change calcium fully to dissolve as uniform colloidal sol;
3)Colloidal sol made from step 2 is placed into centrifugation degasser and deaerated, and is cooled to 60-65 °C, insulation 24 hours;
4)By colloidal sol made from step 3 with Flat Membrane knifing machine even application on non-woven fabrics base material, coated film thickness control exists 20-120μm;
5)Flat Membrane after film, which is immersed in water-bath, carries out gel, and bath temperature is controlled at 20-25 °C;
6)The processing such as test, be dehydrated after film forming, supporting layer is made;
7)By m-phenylene diamine (MPD), water and neopelex according to quality parts ratio be 1:98:2 ratio is mixed into For mixed liquor one;
8)By pyromellitic trimethylsilyl chloride, n-hexane according to quality parts ratio be 1:99 ratio is well mixed to turn into mixed liquor two;
9)By step 6 obtain be coated with the basement membrane of supporting layer be immersed in 0-30 °C of mixed liquor one soak 1-60 seconds after take Go out;
10)The film that step 9 is obtained applies 0-30 °C of mixed liquor two through Flat Membrane coating machine;
11)The film that step 10 is obtained is immersed in 20-60 °C of pure water, soak time 1-20 hours;
12)Air drying of the film that step 11 is obtained at 20-30 °;
13)The film that step 12 is obtained heats under 50-90 °C, and the composite nanometer filtering film of three-decker is made.
Using above-mentioned technical proposal, the preparation method of composite nanometer filtering film of the invention, formula is simple, and technological operation is convenient, It is easy to industrialized production.Using the technology of the present invention, obtained composite nanometer filtering film has preferable chemical stability and antipollution Property, 97% is more than to magnesium sulfate rejection rate, 85% is more than to sodium chloride rejection.
Embodiment
Below by way of embodiment, the present invention is described in further detail.
The present invention provides a kind of preparation method of composite nanometer filtering film, and the composite nanometer filtering film includes non-woven fabrics basement membrane, positioned at nothing Spin the epilamellar chliorinated polyvinyl chloride supporting layer of cloth and the aromatic polyamides positioned at the chliorinated polyvinyl chloride supporting layer are separated Layer;The preparation method of the composite nanometer filtering film comprises the following steps:
1)It is 12 that chliorinated polyvinyl chloride, dimethylformamide and calcium chloride are pressed into quality parts ratio:18:6 ratio is weighed After mix;
2)The mixed liquor of step 1 is stirred and 70-80 °C is gradually heating to, makes chliorinated polyvinyl chloride, dimethylformamide and chlorine Change calcium fully to dissolve as uniform colloidal sol;
3)Colloidal sol made from step 2 is placed into centrifugation degasser and deaerated, and is cooled to 60-65 °C, insulation 24 hours;
4)By colloidal sol made from step 3 with Flat Membrane knifing machine even application on non-woven fabrics base material, coated film thickness control exists 20-120μm;
5)Flat Membrane after film, which is immersed in water-bath, carries out gel, and bath temperature is controlled at 20-25 °C;
6)The processing such as test, be dehydrated after film forming, supporting layer is made;
7)By m-phenylene diamine (MPD), water and neopelex according to quality parts ratio be 1:98:2 ratio is mixed into For mixed liquor one;
8)By pyromellitic trimethylsilyl chloride, n-hexane according to quality parts ratio be 1:99 ratio is well mixed to turn into mixed liquor two;
9)By step 6 obtain be coated with the basement membrane of supporting layer be immersed in 0-30 °C of mixed liquor one soak 1-60 seconds after take Go out;
10)The film that step 9 is obtained applies 0-30 °C of mixed liquor two through Flat Membrane coating machine;
11)The film that step 10 is obtained is immersed in 20-60 °C of pure water, soak time 1-20 hours;
12)Air drying of the film that step 11 is obtained at 20-30 °;
13)The film that step 12 is obtained heats under 50-90 °C, and the composite nanometer filtering film of three-decker is made.
Using above-mentioned technical proposal, the preparation method of composite nanometer filtering film of the invention, formula is simple, and technological operation is convenient, It is easy to industrialized production.Using the technology of the present invention, obtained composite nanometer filtering film has preferable chemical stability and antipollution Property, 97% is more than to magnesium sulfate rejection rate, 85% is more than to sodium chloride rejection.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.For For the those of ordinary skill in the field, other various forms of changes or change can also be made on the basis of the above description It is dynamic.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change or change thus extended out Among moving still in the protection domain of the invention.

Claims (1)

1. a kind of preparation method of composite nanometer filtering film, it is characterised in that:The composite nanometer filtering film includes non-woven fabrics basement membrane, positioned at nonwoven The epilamellar chliorinated polyvinyl chloride supporting layer of cloth and the aromatic polyamides separating layer positioned at the chliorinated polyvinyl chloride supporting layer; The preparation method of the composite nanometer filtering film comprises the following steps:
1)It is 12 that chliorinated polyvinyl chloride, dimethylformamide and calcium chloride are pressed into quality parts ratio:18:6 ratio is weighed After mix;
2)The mixed liquor of step 1 is stirred and 70-80 °C is gradually heating to, makes chliorinated polyvinyl chloride, dimethylformamide and chlorine Change calcium fully to dissolve as uniform colloidal sol;
3)Colloidal sol made from step 2 is placed into centrifugation degasser and deaerated, and is cooled to 60-65 °C, insulation 24 hours;
4)By colloidal sol made from step 3 with Flat Membrane knifing machine even application on non-woven fabrics base material, coated film thickness control exists 20-120μm;
5)Flat Membrane after film, which is immersed in water-bath, carries out gel, and bath temperature is controlled at 20-25 °C;
6)The processing such as test, be dehydrated after film forming, supporting layer is made;
7)By m-phenylene diamine (MPD), water and neopelex according to quality parts ratio be 1:98:2 ratio is mixed into For mixed liquor one;
8)By pyromellitic trimethylsilyl chloride, n-hexane according to quality parts ratio be 1:99 ratio is well mixed to turn into mixed liquor two;
9)By step 6 obtain be coated with the basement membrane of supporting layer be immersed in 0-30 °C of mixed liquor one soak 1-60 seconds after take Go out;
10)The film that step 9 is obtained applies 0-30 °C of mixed liquor two through Flat Membrane coating machine;
11)The film that step 10 is obtained is immersed in 20-60 °C of pure water, soak time 1-20 hours;
12)Air drying of the film that step 11 is obtained at 20-30 °;
13)The film that step 12 is obtained heats under 50-90 °C, and the composite nanometer filtering film of three-decker is made.
CN201710431105.6A 2017-06-09 2017-06-09 A kind of preparation method of composite nanometer filtering film Pending CN107158971A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN103055715A (en) * 2013-02-04 2013-04-24 北京科泰兴达高新技术有限公司 Composite nanofiltration membrane and preparation method thereof
CN105934271A (en) * 2013-04-10 2016-09-07 南洋理工大学 Nanofiltration membrane and method of manufacturing a nanofiltration membrane

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103055715A (en) * 2013-02-04 2013-04-24 北京科泰兴达高新技术有限公司 Composite nanofiltration membrane and preparation method thereof
CN105934271A (en) * 2013-04-10 2016-09-07 南洋理工大学 Nanofiltration membrane and method of manufacturing a nanofiltration membrane

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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: 20170915

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