CN102909813A - Preparation method of blending modified super-hydrophobic surface - Google Patents
Preparation method of blending modified super-hydrophobic surface Download PDFInfo
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- CN102909813A CN102909813A CN 201210390294 CN201210390294A CN102909813A CN 102909813 A CN102909813 A CN 102909813A CN 201210390294 CN201210390294 CN 201210390294 CN 201210390294 A CN201210390294 A CN 201210390294A CN 102909813 A CN102909813 A CN 102909813A
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Abstract
The invention relates to a preparation method of a blending modified super-hydrophobic surface, which comprises the steps as follows: a, preparing a blend; b, mixing; c, tabletting; d, pressing films; e, laminating and pressing the films; f, conducting interlayer stripping; and g, measuring a contact angle and a roll angle of the super-hydrophobic surface. The preparation method has the benefits that a linear low-density polyethylene/linear low-density polyethylene and linear low-density polyethylene/polypropylene blend super-hydrophobic film is prepared by a simple blending and stripping method, and the preparation method is simple to operate and lower in cost, and can be combined with a calendering process of a polymer for producing various polymer super-hydrophobic films in a large scale and at a low cost.
Description
Technical field
The present invention relates to a kind of preparation method of blending and modifying super hydrophobic surface.
Background technology
Super hydrophobic surface is with a wide range of applications, and has become in recent years the focus of investigation of materials, has developed numerous different raw materials and process.By model analysis, for the relation between surface microstructure and contact angle, hysteresis, the wet face state more deep understanding has been arranged also, for having special surface wellability material, preparation provides certain theoretical direction.
But the practical application of super hydrophobic surface also fails to popularize, and many problems also need to be resolved hurrily.
At first, simple economy, eco-friendly preparation method have to be developed.All relate in the preparation process of most of super hydrophobic surfaces of existing report with expensive low-surface-energy material, reduce the surface energy on surface such as the compound of fluorine-containing or silane, and many methods relate to specific equipment, exacting terms and long cycle, are difficult to use in the preparation of large tracts of land super hydrophobic surface.
Secondly, consider that from the practical application angle intensity and the persistence of existing super hydrophobic surface are poor, so that this surface is restricted in the application of many occasions.The surface micro-structural also because of bad mechanical strength easily by outside destroy, cause the forfeiture of super-hydrophobicity; The surface also may be polluted by oily matter in some occasions or long-term the use in addition, so that the hydrophobicity variation.Exploitation has the recoverable super hydrophobic surface of surface micro-structure and realizes that super two hydrophobic functions (not only hydrophobic but also oleophobic) may be the preferred plan of solution actual application problem.
In addition, consider from the theory analysis angle, for how much patterns, size and surface wettabilities of surface micro-structure, especially be still waiting deeply with the quantitative study that hysteresis is contacted directly.
At last, the application of super hydrophobic surface is still waiting to expand, especially in biological field.Having the growth of bioactivator such as cell, albumen etc. and the interaction between the surface etc. at super hydrophobic surface all will be the content that is worth research.
Summary of the invention
The technical problem to be solved in the present invention is: based on the problems referred to above, the invention provides a kind of preparation method of blending and modifying super hydrophobic surface.
The present invention solves the technical scheme that its technical problem adopts: a kind of preparation method of blending and modifying super hydrophobic surface, and concrete steps are as follows:
A, preparation blend: with LLDPE and LLDPE by ratio of component (45～95%): (5～55%) are hybridly prepared into LLDPE/LLDPE blend, or with LLDPE and polypropylene by ratio of component (45～95%): (5～55%) are hybridly prepared into LLDPE/polypropylene blend;
B, mixing: with the Haake torque rheometer with the LLDPE prepared among a/LLDPE blend or mixing one-tenth sample of LLDPE/polypropylene blend, melting temperature is 195～205 ℃, mixing time is 5～7min, and rotor speed is 55～65r/min;
C, compressing tablet: the LLDPE after mixing among the b/LLDPE blend sample or LLDPE/polypropene blended matter sample be placed on carry out compressing tablet on the opening rubber mixing machine;
D, press mold: regulating mold thickness is 0.9～1.1mm(specification), molding temperature is 195～205 ℃, and the LLDPE that forms behind the compressing tablet among the c/LLDPE blend or LLDPE/polypropylene blend are pressed into LLDPE/linear low-density polyethylene film or LLDPE/polypropylene film by vulcanizing press;
E, stacked press mold: regulating the mould molding temperature is 195～205 ℃, be 2～4min preheating time, dwell time is 55～65s, pressure is 2.9～3.1MPa, with vulcanizing press LLDPE/linear low-density polyethylene film is embossed in linear low-density polyethylene film is stacked, or with vulcanizing press LLDPE/polypropylene film is embossed in polypropylene film is stacked;
F, splitting: with pliers LLDPE/linear low-density polyethylene film and linear low-density polyethylene film that mold pressing among the e has been stacked in are peeled off, obtained the super hydrophobic surface with the LLDPE/linear low-density polyethylene film of filamentary structure; Or with pliers LLDPE/polypropylene film and polypropylene film that mold pressing among the e has been stacked in are peeled off, obtain the super hydrophobic surface with the LLDPE/polypropylene film of filamentary structure;
Contact angle, the roll angle of g, measurement super hydrophobic surface: ratio of component (60～80%): 150 ° of the contact angle ﹥ of the LLDPE of (20～40%)/LLDPE super hydrophobic surface, 10 ° of its roll angle ﹤; Ratio of component (60～80%): 150 ° of the contact angle ﹥ on the LLDPE of (20～40%)/polypropylene super-hydrophobic surface, 10 ° of its roll angle ﹤.
The invention has the beneficial effects as follows: adopt the simple blend stripping means, LLDPE/LLDPE, LLDPE/polypropylene blend based superhydrophobic thin films have been prepared, simple to operate, cost is lower, can combine with the calendering technology of polymer extensive, the various polymer super-hydrophobic films of low-cost production.
Description of drawings
The present invention is further described below in conjunction with accompanying drawing.
Fig. 1 is the scanning electron microscope diagram sheet of the LLDPE/linear low-density polyethylene film surface of ratio of component 90g:10g;
Fig. 2 is the scanning electron microscope diagram sheet of the LLDPE/linear low-density polyethylene film surface of ratio of component 80g:20g;
Fig. 3 is the scanning electron microscope diagram sheet of the LLDPE/linear low-density polyethylene film surface of ratio of component 70g:30g;
Fig. 4 is the scanning electron microscope diagram sheet of the LLDPE/linear low-density polyethylene film surface of ratio of component 60g:40g;
Fig. 5 is that water droplet is in the video interception one of the LLDPE that tilts/linear low-density polyethylene film surface rolling;
Fig. 6 is that water droplet is in the video interception two of the LLDPE that tilts/linear low-density polyethylene film surface rolling;
Fig. 7 is the scanning electron microscope diagram sheet of the LLDPE/polypropylene film surface of ratio of component 90g:10g;
Fig. 8 is the scanning electron microscope diagram sheet of the LLDPE/polypropylene film surface of ratio of component 80g:20g;
Fig. 9 is the scanning electron microscope diagram sheet of the LLDPE/polypropylene film surface of ratio of component 70g:30g;
Figure 10 is the scanning electron microscope diagram sheet of the LLDPE/polypropylene film surface of ratio of component 60g:40g;
Figure 11 is that water droplet is in the video interception one of the LLDPE that tilts/polypropylene film surface rolling;
Figure 12 is that water droplet is in the video interception two of the LLDPE that tilts/polypropylene film surface rolling.
The specific embodiment
The invention will be further described in conjunction with specific embodiments now, and following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1:
Be 100g by amount of the mixture, LLDPE and LLDPE are mixed by 90g:10g or 80g:20g or 70g:30g or 60g:40g or 50g:50g, carry out mixing with LH60 Haake torque rheometer, melting temperature is 200 ℃, mixing time is 6min, rotor speed is 60r/min, and the sample that mixes is placed on compressing tablet on the opening rubber mixing machine, makes LLDPE/LLDPE blend.With vulcanizing press mold pressing LLDPE/linear low density polyethylene (LDPE)/linear low-density polyethylene film of LLDPE blend, mold thickness is 1mm, and molding temperature is 200 ℃.With the stacked press mold of vulcanizing press, molding temperature is 200 ℃ with LLDPE/linear low-density polyethylene film and linear low-density polyethylene film, preheating time 3min, dwell time 60s, pressure are 3MPa.LLDPE/the linear low-density polyethylene film and the linear low-density polyethylene film that are embossed in are together peeled off with pliers, acquisition is with the LLDPE of filamentary structure/LLDPE super hydrophobic surface, and LLDPE/linear low-density polyethylene film is carried out electron-microscope scanning and contact angle, roll angle are measured.
Ratio of component is that the LLDPE/linear low-density polyethylene film surface surface fiber shape structure of 90g:10g is less and sparse, and contact angle is 149 °, shows such as Fig. 1.
Ratio of component be 80g:20g LLDPE/linear low-density polyethylene film surface fiber shape mechanism is large and intensive, there are many passive hangnails on the surface, contact angle is 150.6 °, shows such as Fig. 2.
Ratio of component be 70g:30g LLDPE/linear low-density polyethylene film surface fiber shape mechanism is large and intensive, there are many passive hangnails on the surface, contact angle is 152 °, shows such as Fig. 3.
Ratio of component be 60g:40g LLDPE/linear low-density polyethylene film surface fiber shape mechanism is large and intensive, there are many passive hangnails on the surface, contact angle is 155 °, shows such as Fig. 4.
Ratio of component is that LLDPE/linear low-density polyethylene film two alternate combinations of 50g:50g are tight, can't open, and can not form hydrophobic structure.
As fully visible, when adding LLDPE content was 10g, contact angle was 149 °, and LLDPE/LLDPE surface does not reach super-hydrophobic; When adding LLDPE content at 20g～40g, along with the increase of LLDPE content, surface fiber shape structure is intensive and begin to become large gradually, there are many hangnails on the surface, play a supportive role, 150 ° of contact angle ﹥ have preferably super-hydrophobicity; When adding LLDPE content was increased to 50g, two alternate combinations were tight, almost can't open, and can not form hydrophobic structure.
Be that the LLDPE/linear low-density polyethylene film of 80g:20g or 70g:30g or 60g:40g tilts 7 ° with ratio of component, take the process that water droplet tumbles at film surface with camera, show such as Fig. 5, Fig. 6, very little angle water droplet will tumble from the surface as long as tilt, 10 ° of the roll angle ﹤ that LLDPE/the LLDPE based superhydrophobic thin films presents, film has good ultra-hydrophobicity.
Embodiment 2:
Be 100g by amount of the mixture, LLDPE and polypropylene are mixed by 90g:10g or 80g:20g or 70g:30g or 60g:40g or 50g:50g, carry out mixing with LH60 Haake torque rheometer, melting temperature is 200 ℃, mixing time is 6min, rotor speed is 60r/min, and the sample that mixes is placed on compressing tablet on the opening rubber mixing machine, makes LLDPE/polypropylene blend.With the linear low density polyethylene (LDPE)/polypropylene film of vulcanizing press mold pressing LLDPE/polypropylene blend, mold thickness is 1mm, and molding temperature is 200 ℃.With the stacked press mold of vulcanizing press, molding temperature is 200 ℃ with LLDPE/polypropylene film and polypropylene film, preheating time 3min, dwell time 60s, pressure are 3MPa.LLDPE/the polypropylene film and the polypropylene film that are embossed in are together peeled off with pliers, acquisition is with the LLDPE of filamentary structure/polypropylene super-hydrophobic surface, and LLDPE/polypropylene film is carried out electron-microscope scanning and contact angle, roll angle are measured.
Ratio of component is that the LLDPE/polypropylene film surface surface fiber shape structure of 90g:10g is less and sparse, and contact angle is 145 °, shows such as Fig. 7.
Ratio of component be 80g:20g LLDPE/polypropylene film surface fiber shape mechanism is large and intensive, there are many passive hangnails on the surface, contact angle is 150.6 °, shows such as Fig. 8.
Ratio of component be 70g:30g LLDPE/polypropylene film surface fiber shape mechanism is large and intensive, there are many passive hangnails on the surface, contact angle is 152 °, shows such as Fig. 9.
Ratio of component be 60g:40g LLDPE/polypropylene film surface fiber shape mechanism is large and intensive, there are many passive hangnails on the surface, contact angle is 152 °, shows such as Figure 10.
Ratio of component is that LLDPE/polypropylene film two alternate combinations of 50g:50g are tight, can't open, and can not form hydrophobic structure.
As fully visible, when the adding polypropylene content was 10g, contact angle was 145 °, and it is super-hydrophobic that LLDPE/polypropylene surface does not reach; When adding polypropylene content at 20g～40g, along with the increase of polypropylene content, surface fiber shape structure is intensive and begin to become large gradually, and there are many hangnails on the surface, plays a supportive role, and 150 ° of contact angle ﹥ have preferably super-hydrophobicity; When the adding polypropylene content was increased to 50g, two alternate combinations were tight, almost can't open, and can not form hydrophobic structure.
Be that the LLDPE/polypropylene blend film of 80g:20g or 70g:30g or 60g:40g tilts 7 ° with ratio of component, take the process that water droplet tumbles at film surface with camera, show such as Figure 11, Figure 12, very little angle water droplet will tumble from the surface as long as tilt, LLDPE/polypropylene super-hydrophobic film presents 10 ° of roll angle ﹤, and film has good ultra-hydrophobicity.
Take above-mentioned foundation desirable embodiment of the present invention as enlightenment, by above-mentioned description, the relevant staff can in the scope that does not depart from this invention technological thought, carry out various change and modification fully.The technical scope of this invention is not limited to the content on the specification, must determine its technical scope according to the claim scope.
Claims (1)
1. the preparation method of a blending and modifying super hydrophobic surface, it is characterized in that: concrete steps are as follows:
A, preparation blend: with LLDPE and LLDPE by ratio of component (45～95%): (5～55%) are hybridly prepared into LLDPE/LLDPE blend, or with LLDPE and polypropylene by ratio of component (45～95%): (5～55%) are hybridly prepared into LLDPE/polypropylene blend;
B, mixing: with the Haake torque rheometer with the LLDPE prepared among a/LLDPE blend or mixing one-tenth sample of LLDPE/polypropylene blend, melting temperature is 195～205 ℃, mixing time is 5～7min, and rotor speed is 55～65r/min;
C, compressing tablet: the LLDPE after mixing among the b/LLDPE blend sample or LLDPE/polypropene blended matter sample be placed on carry out compressing tablet on the opening rubber mixing machine;
D, press mold: regulating mold thickness is 0.9～1.1mm(specification), molding temperature is 195～205 ℃, and the LLDPE that forms behind the compressing tablet among the c/LLDPE blend or LLDPE/polypropylene blend are pressed into LLDPE/linear low-density polyethylene film or LLDPE/polypropylene film by vulcanizing press;
E, stacked press mold: regulating the mould molding temperature is 195～205 ℃, be 2～4min preheating time, dwell time is 55～65s, pressure is 2.9～3.1MPa, with vulcanizing press LLDPE/linear low-density polyethylene film is embossed in linear low-density polyethylene film is stacked, or with vulcanizing press LLDPE/polypropylene film is embossed in polypropylene film is stacked;
F, splitting: with pliers LLDPE/linear low-density polyethylene film and linear low-density polyethylene film that mold pressing among the e has been stacked in are peeled off, obtained the super hydrophobic surface with the LLDPE/linear low-density polyethylene film of filamentary structure; Or with pliers LLDPE/polypropylene film and polypropylene film that mold pressing among the e has been stacked in are peeled off, obtain the super hydrophobic surface with the LLDPE/polypropylene film of filamentary structure;
Contact angle, the roll angle of g, measurement super hydrophobic surface: ratio of component (60～80%): 150 ° of the contact angle ﹥ of the LLDPE of (20～40%)/LLDPE super hydrophobic surface, 10 ° of its roll angle ﹤; Ratio of component (60～80%): 150 ° of the contact angle ﹥ on the LLDPE of (20～40%)/polypropylene super-hydrophobic surface, 10 ° of its roll angle ﹤.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210390294 CN102909813A (en) | 2012-10-15 | 2012-10-15 | Preparation method of blending modified super-hydrophobic surface |
| CN201310072009.9A CN103231528B (en) | 2012-10-15 | 2013-03-06 | Method for preparing super-hydrophobic surface by composite membrane interlayer stripping |
| CN201310072565.6A CN103144237B (en) | 2012-10-15 | 2013-03-06 | Preparation method of blend-modified ultrahydrophobic surface |
| CN201310071988.6A CN103231527B (en) | 2012-10-15 | 2013-03-06 | Preparation method of surface-foaming super-hydrophobic surface |
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| CN 201210390294 CN102909813A (en) | 2012-10-15 | 2012-10-15 | Preparation method of blending modified super-hydrophobic surface |
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| CN201310071988.6A Active CN103231527B (en) | 2012-10-15 | 2013-03-06 | Preparation method of surface-foaming super-hydrophobic surface |
| CN201310072009.9A Expired - Fee Related CN103231528B (en) | 2012-10-15 | 2013-03-06 | Method for preparing super-hydrophobic surface by composite membrane interlayer stripping |
| CN201310072565.6A Active CN103144237B (en) | 2012-10-15 | 2013-03-06 | Preparation method of blend-modified ultrahydrophobic surface |
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| CN201310072009.9A Expired - Fee Related CN103231528B (en) | 2012-10-15 | 2013-03-06 | Method for preparing super-hydrophobic surface by composite membrane interlayer stripping |
| CN201310072565.6A Active CN103144237B (en) | 2012-10-15 | 2013-03-06 | Preparation method of blend-modified ultrahydrophobic surface |
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| CN105111473A (en) * | 2015-09-09 | 2015-12-02 | 哈尔滨工业大学 | Preparing method for super-hydrophobic LDPE film |
| CN105172120A (en) * | 2015-10-12 | 2015-12-23 | 青岛大学 | Preparation method of polypropylene super-hydrophobic surface with rolling angle controllable |
| CN105196577A (en) * | 2015-10-12 | 2015-12-30 | 青岛大学 | Rolling angle controllable linear low-density polyethylene super-hydrophobic sheet/container and preparation method thereof |
| CN105235294A (en) * | 2015-10-12 | 2016-01-13 | 青岛大学 | Low-density polyethylene super hydrophobic sheets/containers with controllable rolling angle and preparation method thereof |
| CN105346146A (en) * | 2015-10-12 | 2016-02-24 | 青岛大学 | High-density polyethylene super-hydrophobic sheet material/container with controllable roll angle and preparation method thereof |
| WO2018045621A1 (en) * | 2016-09-09 | 2018-03-15 | 东南大学 | Transferable wear-resistant flexible super-hydrophobic film and preparation method therefor |
| CN113491956A (en) * | 2021-07-15 | 2021-10-12 | 河南工程学院 | LLDPE oil-water separation membrane and preparation method and application thereof |
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| CN105269727A (en) * | 2015-11-21 | 2016-01-27 | 青岛科技大学 | Preparation method for flexible super-hydrophobic material based on thermoplastic vulcanized rubber |
| CN107090087B (en) * | 2017-05-12 | 2020-04-21 | 郑州大学 | Method for preparing adhesion-controllable PLA (polylactic acid) super-hydrophobic film by using solvent-non-solvent assisted microphase separation method |
| CN110682499B (en) * | 2019-11-07 | 2020-06-26 | 四川大学 | Polyethylene hydrophobic material and preparation method thereof |
| CN112934012B (en) * | 2021-01-28 | 2022-08-19 | 华北电力大学 | Tubular ceramic membrane surface super-hydrophobic modification method based on polytetrafluoroethylene |
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| DE3689520T2 (en) * | 1985-11-07 | 1994-04-28 | Showa Denko Kk | TRANSPARENT, HIGH DENSITY POLYETHYLENE FILM AND THEIR PRODUCTION. |
| JPH0516159A (en) * | 1991-07-12 | 1993-01-26 | Shin Etsu Chem Co Ltd | Manufacture of resin membrane |
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| BRPI0720817A2 (en) * | 2007-01-26 | 2014-03-04 | Guangdong Decro Packaga Films Co Ltd | BIAXIALLY SUITABLE ORIENTED POLYPROPYLENE FILM FOR PAPER FREE GLAMING AND METHOD FOR PREPARING A SUITABLE ORIENTED POLYPROPYLENE FILM FOR PAPER |
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| CN101768396B (en) * | 2009-01-04 | 2012-09-26 | 中国科学院化学研究所 | Blending modified polypropylene super-hydrophobic coating or film with controllable rolling angle and preparation method thereof |
| CN101537682B (en) * | 2009-03-16 | 2011-06-29 | 浙江工业大学 | Method for preparing superhydrophobic surface by using nano-particles for assisting micromolding |
| CN101851069B (en) * | 2010-02-11 | 2012-05-30 | 浙江工业大学 | Method for preparing polymer super-hydrophobic surface by using screen template method |
| CN101817951B (en) * | 2010-05-11 | 2012-02-08 | 赵健 | Waterproof roll material with improved ageing resistance and preparation method thereof |
| CN103370143B (en) * | 2010-12-17 | 2015-10-07 | 纤维素技术公司 | A kind of new method of producing super hydrophobic surface |
| CN102173156A (en) * | 2011-03-11 | 2011-09-07 | 佛山塑料集团股份有限公司 | Biaxial tension polyethylene film and preparation method thereof |
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- 2013-03-06 CN CN201310071988.6A patent/CN103231527B/en active Active
- 2013-03-06 CN CN201310072009.9A patent/CN103231528B/en not_active Expired - Fee Related
- 2013-03-06 CN CN201310072565.6A patent/CN103144237B/en active Active
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| CN105111473A (en) * | 2015-09-09 | 2015-12-02 | 哈尔滨工业大学 | Preparing method for super-hydrophobic LDPE film |
| CN105172120A (en) * | 2015-10-12 | 2015-12-23 | 青岛大学 | Preparation method of polypropylene super-hydrophobic surface with rolling angle controllable |
| CN105196577A (en) * | 2015-10-12 | 2015-12-30 | 青岛大学 | Rolling angle controllable linear low-density polyethylene super-hydrophobic sheet/container and preparation method thereof |
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| CN105346146A (en) * | 2015-10-12 | 2016-02-24 | 青岛大学 | High-density polyethylene super-hydrophobic sheet material/container with controllable roll angle and preparation method thereof |
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| CN105235294B (en) * | 2015-10-12 | 2016-10-19 | 青岛大学 | Super-hydrophobic sheet material/container of Low Density Polyethylene that roll angle is controlled and preparation method thereof |
| CN105196577B (en) * | 2015-10-12 | 2016-10-19 | 青岛大学 | Super-hydrophobic sheet material/container of linear low density polyethylene that roll angle is controlled and preparation method thereof |
| WO2018045621A1 (en) * | 2016-09-09 | 2018-03-15 | 东南大学 | Transferable wear-resistant flexible super-hydrophobic film and preparation method therefor |
| CN113491956A (en) * | 2021-07-15 | 2021-10-12 | 河南工程学院 | LLDPE oil-water separation membrane and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103144237A (en) | 2013-06-12 |
| CN103144237B (en) | 2015-04-01 |
| CN103231527A (en) | 2013-08-07 |
| CN103231528A (en) | 2013-08-07 |
| CN103231527B (en) | 2015-04-01 |
| CN103231528B (en) | 2015-04-01 |
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Application publication date: 20130206 |