CN104722217A - Support-free nylon 66 microporous film and preparation method thereof - Google Patents
Support-free nylon 66 microporous film and preparation method thereof Download PDFInfo
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- CN104722217A CN104722217A CN201310723430.1A CN201310723430A CN104722217A CN 104722217 A CN104722217 A CN 104722217A CN 201310723430 A CN201310723430 A CN 201310723430A CN 104722217 A CN104722217 A CN 104722217A
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Abstract
The invention relates to a support-free nylon 66 microporous film and a preparation method thereof. The support-free nylon 66 microporous film is characterized in that the hole diameter is 0.01-20 microns, and the thickness is 30-200 microns. The preparation method comprises the following steps: (1) preparing a casting film liquid, namely firstly dissolving nylon 66 into a solvent, adding an additive, and adequately stirring at 5-40 DEG C so as to form the uniform and stable casting film liquid; and (2) carrying out phase inversion film formation, namely casting the casting film liquid to a stainless steel roller, scraping the film by virtue of a scraping knife, after standing for 1-400 seconds in air, sequentially carrying out first coagulating bath, second coagulating bath and third coagulating bath, carrying out hot water bath washing, and drying a film sheet, so as to obtain the support-free nylon 66 microporous film, wherein the interval between the scraping knife and the stainless steel roller is 30-300 microns. Compared with the prior art, the support-free nylon 66 microporous film has the advantages that the extraction is thorough, the particle size is uniform, the filter precision and the filter efficiency are relatively high, the product performance is stable and the like; the support-free nylon 66 microporous film can be applied to produced in a continuous large-scale manner.
Description
Technical field
The present invention relates to food, beverage, biochemical pharmacy, the contour terminal membrane application of health care, especially relate to a kind of without Supported Nylon 66 microporous barrier and preparation method thereof.
Background technology
Nylon66 fiber microporous barrier is applied in a lot of fields because of its distinctive organic solvent resistance and the diluted alkaline of resistance to diluted acid performance.My company has succeeded in developing reinforced PA66 microporous barrier, has filled up domestic blank.But in electronics, biochemical pharmacy, the contour terminal membrane application of health care, more and more harsher to the requirement of film, require the stripping of film, the extraction of film inner additive and solvent will meet professional standard completely, and all there is problem more or less owing to there being polyester backing material at film stripping, extraction this respect in existing film product, this project adopts unique filming technology condition, and product is had, and extraction is thorough, flux is large, filtering accuracy high.
Summary of the invention
Object of the present invention is exactly provide a kind of without Supported Nylon 66 microporous barrier and preparation method thereof to overcome defect that above-mentioned prior art exists.
Object of the present invention can be achieved through the following technical solutions: a kind of without Supported Nylon 66 microporous barrier, it is characterized in that, the aperture of this microporous barrier is 0.01 ~ 20 μm, and thickness is 30 ~ 200 μm.
Without a preparation method for Supported Nylon 66 microporous barrier, it is characterized in that, the method comprises the following steps:
1) formula of casting solution: first nylon66 fiber is dissolved in a solvent, and add additive, at 5 ~ 40 DEG C, fully stir the casting solution becoming stable homogeneous, wherein the content of nylon66 fiber in casting solution is 10 ~ 35wt%, and the content of additive in casting solution is 10 ~ 30wt%:
2) inversion of phases film forming: by casting solution curtain coating on stainless steel drum, use scraper knifing, gap between scraper and stainless steel drum is 30-300 μm, after leaving standstill 1 ~ 400 second in atmosphere, namely obtain described without Supported Nylon 66 microporous barrier after diaphragm being dried enter hot bath cleaning successively after the first coagulating bath, the second gelation and the 3rd coagulating bath after.
The molecular weight of the nylon66 fiber described in step (1) is 12000 ~ 30000:
Described solvent is one or more in dimethyl formamide, dimethylacetylamide, formic acid, methyl alcohol or N-dihydroxy ethyl tallow amine;
Described additive is one or more in lithium chloride, calcium chloride, sodium chloride, polyvinylpyrrolidone, glycerine, water, n-butanol and polyethylene glycol (Mw200 ~ 10000).
The first coagulating bath described in step (2) is the aqueous solution containing additive, described additive is one or more in dimethylacetylamide, dimethyl formamide, dimethyl sulfoxide (DMSO), formic acid, methyl alcohol or N-dihydroxy ethyl tallow amine, its mass concentration in coagulating bath is 0 ~ 80%, coagulation bath temperature is 5 ~ 70 DEG C, and diaphragm is 1 ~ 30 minute in this coagulating bath time of staying.
The second gelation described in step (2) is the aqueous solution containing additive, described additive is one or more of dimethylacetylamide, dimethyl formamide, dimethyl sulfoxide (DMSO), formic acid, methyl alcohol or N-dihydroxy ethyl tallow amine, its mass concentration in coagulating bath is 0 ~ 30%, coagulation bath temperature is 10 ~ 50 DEG C, and diaphragm is 1 ~ 15 minute in this coagulating bath time of staying.
The 3rd coagulating bath described in step (2) is pure water coagulating bath, coagulation bath temperature 10 ~ 50 DEG C, and diaphragm is 1 ~ 15 minute in this coagulating bath time of staying.
Heating bath temperature described in step (2) is 70-95 DEG C, and the diaphragm time of staying is 1 ~ 15 minute.
Bake out temperature described in step (2) is 80-100 DEG C, and the diaphragm time of staying is 1 ~ 20 minute.
Standing in atmosphere relative air humidity described in step (2) is 30 ~ 100%.
Casting solution temperature described in step (2) is 5-40 DEG C.
Compared with prior art, the present invention has the following advantages:
(1) to residual solvent, additive extraction in fenestra thoroughly;
(2) filtering accuracy is high, even aperture distribution, filter efficiency are high;
(3) can be applicable to serialization large-scale production, properties of product are stablized.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
Without a preparation method for Supported Nylon 66 microporous barrier, the method comprises the following steps:
By 140 grams of nylon 66 resins, molecular weight is that 23000,150 grams of additive combination components are dissolved in 610 grams of formic acid and become casting solution under 26 DEG C of conditions.By casting solution standing and defoaming about 24 hours, then evenly scraped after scraper on dull and stereotyped steel plate by casting solution, the gap between scraper was 200 microns, successively by three road coagulating baths, the last drying and shaping film forming of hot bath after one section of humidity is 75% passage.Wherein in the first coagulating bath, formic acid content is 25wt%, and temperature is 25 DEG C, 10 minutes time of staying; In the second gelation, formic acid content is 15wt%, and temperature is 20 DEG C, 5 minutes time of staying; 3rd coagulating bath pure water coagulating bath, temperature is 30 DEG C, 5 minutes time of staying: hot pure water bath temperature is 80 DEG C, 5 minutes time of staying; Bake out temperature is 90 DEG C, 10 minutes time of staying.Adopting 25 DEG C of pure water to be the first bubble point pressure of tested media is 0.26MPa, and pure water flux is 4ml/cm
2(Δ P=0.02MPa, diaphragm area is 20cm to min
2).
Embodiment 2
Without a preparation method for Supported Nylon 66 microporous barrier, the method comprises the following steps:
By 160 grams of nylon 66 resins, molecular weight is that 23000,140 grams of additive combination components are dissolved in 610 grams of formic acid and become casting solution under 18 DEG C of conditions.By casting solution standing and defoaming about 24 hours, then evenly scraped after scraper on dull and stereotyped steel plate by casting solution, the gap between scraper was 200 microns, successively by three road coagulating baths, the last drying and shaping film forming of hot bath after one section of humidity is 75% passage.Wherein in the first coagulating bath, formic acid content is 25wt%, and temperature is 25 DEG C, 10 minutes time of staying; In the second gelation, formic acid content is 15wt%, and temperature is 20 DEG C, 5 minutes time of staying; 3rd coagulating bath pure water coagulating bath, temperature is 30 DEG C, 5 minutes time of staying; Hot pure water bath temperature is 90 DEG C, 5 minutes time of staying; Bake out temperature is 90 DEG C, 10 minutes time of staying.Adopting 25 DEG C of pure water to be the first bubble point pressure of tested media is 0.35MPa, and pure water flux is 2.5ml/cm
2(Δ P=0.02MPa, diaphragm area is 20cm to min
2).
Embodiment 3
Without a preparation method for Supported Nylon 66 microporous barrier, the method comprises the following steps:
1) formula of casting solution: first by molecular weight be 12000 nylon66 fiber be dissolved in solvent dimethylformamide, and add additive lithium chloride, at 5 ~ 40 DEG C, abundant stirring becomes the casting solution of stable homogeneous, wherein the content of nylon66 fiber in casting solution is 10 ~ 35wt%, and the content of additive in casting solution is 10 ~ 30wt%:
2) inversion of phases film forming: be that 5 DEG C of casting solution curtain coatings are on stainless steel drum by temperature, use scraper knifing, gap between scraper and stainless steel drum is 30 μm, be leave standstill after 1 second in the air of 30% in relative humidity, enter after 70 DEG C of hot baths clean 15 minutes successively after the first coagulating bath, the second gelation and the 3rd coagulating bath, namely obtain described without Supported Nylon 66 microporous barrier after 80 DEG C, diaphragm is dried 20 minutes.
The first described coagulating bath is the aqueous solution, and coagulation bath temperature is 5 DEG C, and diaphragm is 30 minutes in this coagulating bath time of staying.
Described the second gelation is the aqueous solution containing additive, and described additive is dimethylacetylamide, and its mass concentration in coagulating bath is 30%, and coagulation bath temperature is 10 DEG C, and diaphragm is 15 minutes in this coagulating bath time of staying.
The 3rd described coagulating bath is pure water coagulating bath, coagulation bath temperature 10 DEG C, and diaphragm is 15 minutes in this coagulating bath time of staying.
Gained is 0.01 ~ 20 μm without the aperture of Supported Nylon 66 microporous barrier, and thickness is 30 ~ 200 μ n.
Embodiment 4
Without a preparation method for Supported Nylon 66 microporous barrier, the method comprises the following steps:
1) formula of casting solution: first by molecular weight be 30000 nylon66 fiber be dissolved in solvent methanol, and add additive glycerine, at 5 ~ 40 DEG C, abundant stirring becomes the casting solution of stable homogeneous, wherein the content of nylon66 fiber in casting solution is 10 ~ 35wt%, and the content of additive in casting solution is l0 ~ 30wt%:
2) inversion of phases film forming: be that 40 DEG C of casting solution curtain coatings are on stainless steel drum by temperature, use scraper knifing, gap between scraper and stainless steel drum is 300 μm, be leave standstill after 400 seconds in the air of 100% in relative humidity, enter after 95 DEG C of hot baths clean 1 minute successively after the first coagulating bath, the second gelation and the 3rd coagulating bath, namely obtain described without Supported Nylon 66 microporous barrier after 100 DEG C, diaphragm is dried 1 minute.
The first described coagulating bath is the aqueous solution containing additive, and described additive is dimethyl sulfoxide (DMSO), and its mass concentration in coagulating bath is 80%, and coagulation bath temperature is 70 DEG C, and diaphragm is 1 minute in this coagulating bath time of staying.
Described the second gelation is the aqueous solution, and coagulation bath temperature is 50 DEG C, and diaphragm is 1 minute in this coagulating bath time of staying.
The 3rd described coagulating bath is pure water coagulating bath, coagulation bath temperature 50 DEG C, and diaphragm is 1 minute in this coagulating bath time of staying.
Gained is 0.01 ~ 20 μm without the aperture of Supported Nylon 66 microporous barrier, and thickness is 30 ~ 200 μm.
Claims (10)
1. without Supported Nylon 66 microporous barrier, it is characterized in that, the aperture of this microporous barrier is 0.01 ~ 20 μm, and thickness is 30 ~ 200 μm.
2., as claimed in claim 1 without a preparation method for Supported Nylon 66 microporous barrier, it is characterized in that, the method comprises the following steps:
1) formula of casting solution: first nylon66 fiber is dissolved in a solvent, and add additive, at 5 ~ 40 DEG C, fully stir the casting solution becoming stable homogeneous, wherein the content of nylon66 fiber in casting solution is 10 ~ 35wt%, and the content of additive in casting solution is 10 ~ 30wt%:
2) inversion of phases film forming: by casting solution curtain coating on stainless steel drum, use scraper knifing, gap between scraper and stainless steel drum is 30-300 μm, after leaving standstill 1 ~ 400 second in atmosphere, namely obtain described without Supported Nylon 66 microporous barrier after diaphragm being dried enter hot bath cleaning successively after the first coagulating bath, the second gelation and the 3rd coagulating bath after.
3. the preparation method without Supported Nylon 66 microporous barrier according to claim 2, is characterized in that, the molecular weight of the nylon66 fiber described in step (1) is 12000 ~ 30000;
Described solvent is one or more in dimethyl formamide, dimethylacetylamide, formic acid, methyl alcohol or N-dihydroxy ethyl tallow amine;
Described additive is one or more in lithium chloride, calcium chloride, sodium chloride, polyvinylpyrrolidone, glycerine, water, n-butanol and polyethylene glycol (Mw200 ~ 10000).
4. the preparation method without Supported Nylon 66 microporous barrier according to claim 2, it is characterized in that, the first coagulating bath described in step (2) is the aqueous solution containing additive, described additive is one or more in dimethylacetylamide, dimethyl formamide, dimethyl sulfoxide (DMSO), formic acid, methyl alcohol or N-dihydroxy ethyl tallow amine, its mass concentration in coagulating bath is 0 ~ 80%, coagulation bath temperature is 5 ~ 70 DEG C, and diaphragm is 1 ~ 30 minute in this coagulating bath time of staying.
5. the preparation method without Supported Nylon 66 microporous barrier according to claim 2, it is characterized in that, the second gelation described in step (2) is the aqueous solution containing additive, described additive is one or more of dimethylacetylamide, dimethyl formamide, dimethyl sulfoxide (DMSO), formic acid, methyl alcohol or N-dihydroxy ethyl tallow amine, its mass concentration in coagulating bath is 0 ~ 30%, coagulation bath temperature is 10 ~ 50 DEG C, and diaphragm is 1 ~ 15 minute in this coagulating bath time of staying.
6. the preparation method without Supported Nylon 66 microporous barrier according to claim 2, it is characterized in that, the 3rd coagulating bath described in step (2) is pure water coagulating bath, coagulation bath temperature 10 ~ 50 DEG C, and diaphragm is 1 ~ 15 minute in this coagulating bath time of staying.
7. the preparation method without Supported Nylon 66 microporous barrier according to claim 2, is characterized in that, the heating bath temperature described in step (2) is 70-95 DEG C, and the diaphragm time of staying is 1 ~ 15 minute.
8. the preparation method without Supported Nylon 66 microporous barrier according to claim 2, is characterized in that, the bake out temperature described in step (2) is 80-100 DEG C, and the diaphragm time of staying is 1 ~ 20 minute.
9. the preparation method without Supported Nylon 66 microporous barrier according to claim 2, is characterized in that, the standing in atmosphere relative air humidity described in step (2) is 30 ~ 100%.
10. the preparation method without Supported Nylon 66 microporous barrier according to claim 2, is characterized in that, the casting solution temperature described in step (2) is 5-40 DEG C.
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| CN201310723430.1A CN104722217A (en) | 2013-12-24 | 2013-12-24 | Support-free nylon 66 microporous film and preparation method thereof |
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| CN201310723430.1A CN104722217A (en) | 2013-12-24 | 2013-12-24 | Support-free nylon 66 microporous film and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106362599A (en) * | 2016-08-29 | 2017-02-01 | 无锡零界净化设备有限公司 | Preparation method of supporting-layer-free micro-porous flat plate filter membrane |
| CN107213799A (en) * | 2017-08-03 | 2017-09-29 | 东北林业大学 | A kind of preparation method for the super hydrophilic stalk coextrusion nylon film superoleophobic under water for being capable of oil-water separation emulsion |
| CN108211799A (en) * | 2017-12-27 | 2018-06-29 | 浙江海洋大学 | A kind of preparation method of the PA66 ultrafiltration membranes of high intensity |
| CN110799261A (en) * | 2017-06-28 | 2020-02-14 | 3M创新有限公司 | Polyamide flat sheet membrane with microporous surface structure for trapping nanoparticles |
| CN111603948A (en) * | 2020-05-21 | 2020-09-01 | 杭州科百特科技有限公司 | Nylon membrane and preparation method and application thereof |
| CN111603946A (en) * | 2020-05-21 | 2020-09-01 | 杭州科百特科技有限公司 | Nylon membrane and preparation method and application thereof |
| CN111603947A (en) * | 2020-05-21 | 2020-09-01 | 杭州科百特科技有限公司 | Nylon membrane with support and preparation method and application thereof |
| CN112619449A (en) * | 2020-12-16 | 2021-04-09 | 杭州科百特科技有限公司 | Nylon membrane and preparation method and application thereof |
| CN116531962A (en) * | 2023-07-06 | 2023-08-04 | 迈博瑞生物膜技术（南通）有限公司 | Polyamide microfiltration membrane and preparation method thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106362599A (en) * | 2016-08-29 | 2017-02-01 | 无锡零界净化设备有限公司 | Preparation method of supporting-layer-free micro-porous flat plate filter membrane |
| CN110799261A (en) * | 2017-06-28 | 2020-02-14 | 3M创新有限公司 | Polyamide flat sheet membrane with microporous surface structure for trapping nanoparticles |
| CN110799261B (en) * | 2017-06-28 | 2022-06-07 | 3M创新有限公司 | Polyamide flat sheet membrane with microporous surface structure for trapping nanoparticles |
| CN107213799A (en) * | 2017-08-03 | 2017-09-29 | 东北林业大学 | A kind of preparation method for the super hydrophilic stalk coextrusion nylon film superoleophobic under water for being capable of oil-water separation emulsion |
| CN107213799B (en) * | 2017-08-03 | 2019-08-09 | 东北林业大学 | A kind of preparation method of super hydrophilic underwater superoleophobic stalk coextrusion nylon film that capableing of oil-water separation lotion |
| CN108211799B (en) * | 2017-12-27 | 2021-03-05 | 浙江海洋大学 | Preparation method of high-strength PA66 ultrafiltration membrane |
| CN108211799A (en) * | 2017-12-27 | 2018-06-29 | 浙江海洋大学 | A kind of preparation method of the PA66 ultrafiltration membranes of high intensity |
| CN111603946A (en) * | 2020-05-21 | 2020-09-01 | 杭州科百特科技有限公司 | Nylon membrane and preparation method and application thereof |
| CN111603947A (en) * | 2020-05-21 | 2020-09-01 | 杭州科百特科技有限公司 | Nylon membrane with support and preparation method and application thereof |
| CN111603948A (en) * | 2020-05-21 | 2020-09-01 | 杭州科百特科技有限公司 | Nylon membrane and preparation method and application thereof |
| CN111603948B (en) * | 2020-05-21 | 2023-06-30 | 杭州科百特科技有限公司 | Nylon membrane and preparation method and application thereof |
| CN111603947B (en) * | 2020-05-21 | 2023-08-01 | 杭州科百特科技有限公司 | Nylon membrane with support and preparation method and application thereof |
| CN112619449A (en) * | 2020-12-16 | 2021-04-09 | 杭州科百特科技有限公司 | Nylon membrane and preparation method and application thereof |
| CN116531962A (en) * | 2023-07-06 | 2023-08-04 | 迈博瑞生物膜技术（南通）有限公司 | Polyamide microfiltration membrane and preparation method thereof |
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Application publication date: 20150624 |