CN105196560A - Method for preparing self-cleaning anti-icing rubber surface by use of waste silicone rubber product - Google Patents
Method for preparing self-cleaning anti-icing rubber surface by use of waste silicone rubber product Download PDFInfo
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Abstract
The invention relates to a method for preparing a self-cleaning anti-icing rubber surface by use of a waste silicone rubber product and belongs to the technical field of surface chemistry. The method comprises the following steps: fully combusting a waste silicone rubber product; grinding obtained combustion products into powder; spreading the powder on a well-shaped mixing rubber surface; placing rubber on which the powder is spread into a die, and performing high-temperature vulcanization shaping in a press vulcanizer; after demoulding, cleaning to obtain a super-hydrophobic rubber surface. The method is simple and convenient, realizes waste utilization, is environment-friendly, dispenses with a special processing instrument and therefore is low in cost. The manufactured super-hydrophobic surface adopts a micro/nano dual structure, and a micro bulge structure has high super-hydrophobicity, self-cleaning capability and favorable mechanical stability, has a favorable application prospect and is expected to realize industrial production.
Description
Technical field
The present invention relates to a kind of use and discard the method that silastic product prepares automatically cleaning freezing rubber surface, belong to technical field of surface chemistry.
Background technology
The biology that researcher is subject to occurring in nature such as the leaf of lotus leaf surface, paddy rice, the pin of water skipper etc. inspire research super hydrophobic surface, and the contact angle of water are reached more than 150 ° and the surface wetting phenomena that roll angle is less than 10 ° calls lotus leaf effect (lotuseffect).Research shows have two kinds of factors to affect surface wettability, surface chemistry composition and special micro-geometrical structure.Through the research of decades, researcher proposes different theoretical models to explain the impact of surface texture on material surface wettability, wherein the most typical, foremost is the not exclusively wetting model of Wenzel complete wetting model and Cassie-Baxter, and the further research of the proposition of these two models rear surface wettability for it provides very important theoretical foundation.The people such as Laforte in 2002 proposes the effect that super-hydrophobic coat may have the adhesion reducing ice first time, thus has promoted the application (Howasolidcoatingcanreducetheadhesionoficeonastructure.20 02) of super hydrophobic surface on anti-freeze.Li Hui etc. to low surface energy coat in the detailed summary of the application in ice-covering-proof field, point out that this type coating is that main body is formed (from surface chemistry to functionalized surface [J] primarily of fluorine-containing, silicone based low surface energy polymeric, chemical progress, 2012).Current researcher obtains the super hydrophobic surface with automatically cleaning and freezing performance mainly through the roughness and reduction its surface energy two aspects increasing surface, and then develops many methods preparing coarse structure super-hydrophobic automatic cleaning surface.Comprising etching method, gel method, electrochemical process, template etc.But these preparation method's process complexities and triviality limit their large-scale application.
General General Purpose Rubber surface is due to electrostatic interaction, often adsorb a lot of dust and foul, liquid can be involved in its inside dust and foul when surface tumbles, but because the hydrophobicity on common material surface is poor, thus indrawn dust and foul can accumulate in material surface again again, and super hydrophobic surface has excellent hydrophobicity and low Adhesion property, liquid is very little at the contact surface of super hydrophobic surface, contact angle is very large, can tumble rapidly, thus dust and foul are taken away, reach self-cleaning object and effect.Some are used in the rubber of outdoor facilities, and as high-tension bus-bar, the surface ice sheet that easily knot is thick in the environment of cold wet such as conveyer belt is difficult to remove.If rubber surface is super-hydrophobic, the effect of making ice frosting can be reached, thus ensure safe operation.
Summary of the invention
The object of the invention is to overcome above-mentioned weak point, a kind of method providing use to discard silastic product to prepare automatically cleaning freezing rubber surface.
According to technical scheme provided by the invention, a kind of use discards the method that silastic product prepares automatically cleaning freezing rubber surface, and step is as follows:
(1) burning of discarded silicon rubber: silastic product Thorough combustion will be discarded, then by gained combustion product grind into powder;
(2) shaping: obtained for step (1) powder to be laid in the mixing of rubber of forming on the surface, the rubber sprinkled with powder is put into mould;
(3) hot-press vulcanization: sulfidization molding in compression molding instrument;
(4) demoulding post processing: mold takes out the rubber after hot-press vulcanization, with ethanol and washed with de-ionized water surface, can form one deck super hydrophobic surface on rubber surface surface after oven dry.
Described use discards the method that silastic product prepares automatically cleaning freezing rubber surface, and concrete steps are:
(1) burning of discarded silicon rubber: will discard silastic product in Muffle furnace at 300-600 DEG C Thorough combustion to burn 5-15min, heating rate is 1-3 DEG C/min; Then by gained combustion product grind into powder, described powder diameter is distributed between 100-1000nm;
(2) shaping: obtained for step (1) powder screen cloth is sprinkled evenly be laid in forming mixing of rubber on the surface, the thickness of powder bed is 0.2-1mm, then the rubber sprinkled with powder is put into mould;
(3) hot-press vulcanization: by step (2) gained material sulfidization molding in compression molding instrument; Curing temperature is 145-180 DEG C, and sulfide stress is 12-16MPa, the hot-press vulcanization time is 30-60min;
(4) demoulding post processing: mold takes out the rubber after hot-press vulcanization, and soak ultrasonic cleaning 5-10min in ethanol, supersonic frequency is 25-50Hz; Then use washed with de-ionized water surface, wash away the powder not being pressed into surface, 30-50 DEG C of oven dry, after oven dry, one deck super hydrophobic surface can be formed at rubber surface, namely obtain automatically cleaning freezing rubber surface.
The mixing of rubber formula of described forming is: rubber 30-100 part, reinforced filling 0-100 part, vulcanizing activator 4-12 part, vulcanizing agent 0.2-5 part, vulcanization accelerator 0.8-5 part, vulcanization accelerator 0.8-5 part, plasticizer 5-25 part, age resistor 1-6 part; By after above-mentioned mixing of materials first at the 40-70 DEG C of 5-10min that plasticates, then after 70-110 DEG C of mixing 10-15min, namely obtain the mixing of rubber of forming.
Described rubber is ethylene propylene diene rubber, butadiene rubber, butadiene-styrene rubber, one or more in natural rubber; Reinforced filling is one or more in N220, N234, N550; Vulcanizing activator is zinc oxide and/or stearic acid; Vulcanizing agent is sulphur and/or DCP; Vulcanization accelerator is one or more in sulfenamide type accelerators CZ, thiazole accelerator DM or thuriam acceserator TMTD; Plasticizer is one or more in coumarone indene resin, aromatic naphtha, carbon 5 Petropols, octyl group phenolic aldehyde BN-2; Age resistor is one or more in anti-aging agent RD, antioxidant 4020 NA, antioxidant MB.
Beneficial effect of the present invention: the present invention adopts the discarded silastic product system in surface to prepare super hydrophobic surface, it is with automatically cleaning freezing function, be a kind of method of simple, convenient, low, the easy processing of cost, the method does not need complicated technology and equipment, and can be mass-produced realization.
The present invention forms one deck super-hydrophobic layer at rubber surface, can take away dust reach self-cleaning object when water droplet drops on while surface tumbles fast.When rubber in the winter time or cold district uses time utilize the performance of super hydrophobic surface extend water freezing time chien shih its before freezing, utilize a series of external force such as wind-force, gravity that water droplet is come off, reduce the contact area of water droplet and rubber surface simultaneously thus reduce rubber surface accumulated ice.
Accompanying drawing explanation
Fig. 1 is the process schematic preparing super hydrophobic surface.
Fig. 2 is General Purpose Rubber surface texture low magnified sweep electron microscope (SEM) image of preparation.
Fig. 3 is super-hydrophobic rubber surface structure low magnified sweep electron microscope (SEM) image of preparation.
Fig. 4 is super-hydrophobic rubber surface structure height magnified sweep electron microscope (SEM) image of preparation.
Detailed description of the invention
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited thereto; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Embodiment 1
(1) the discarded silicon rubber of burning: will discard silastic product 300 DEG C of Thorough combustion 15min in Muffle furnace, heating rate is 1-3 DEG C/min.By gained combustion product grind into powder, the powder diameter of formation is at about 800-1000nm.
(2) powder is shaping together with rubber: previous step gained powder screen cloth is sprinkled evenly tiling 1mm thickness forming mixing of rubber on the surface, the rubber sprinkled with powder is put into mould.
(3) hot-press vulcanization: in compression molding instrument, adopts the conditions of vulcanization of 145 DEG C and 12MPa, hot-press vulcanization 60min.
(4) demoulding post processing: mold takes out the rubber after hot-press vulcanization, is immersed in ethanol medium frequency 30Hz ultrasonic cleaning 5min, and surperficial by washed with de-ionized water.Wash away the powder not being pressed into surface, 30 DEG C of oven dry.One deck super hydrophobic surface can be formed at rubber surface.Whole operating process as shown in Figure 1.
The mixing of rubber formula of described forming is: rubber 30 parts, vulcanizing activator 4 parts, vulcanizing agent 0.2 part, vulcanization accelerator 0.8 part, vulcanization accelerator 0.8 part, 5 parts, plasticizer, 1 part, age resistor; By after above-mentioned mixing of materials first at 40 DEG C of 10min that plasticate, then after 70 DEG C of mixing 15min, namely obtain the mixing of rubber of forming.
Described rubber is ethylene propylene diene rubber, butadiene rubber; Reinforced filling is N220; Vulcanizing activator is zinc oxide and/or stearic acid; Vulcanizing agent is sulphur; Vulcanization accelerator is thiazole accelerator DM and thuriam acceserator TMTD; Plasticizer is carbon 5 Petropols, octyl group phenolic aldehyde BN-2; Age resistor is anti-aging agent RD, antioxidant 4020 NA and antioxidant MB.
Embodiment 2
(1) the discarded silicon rubber of burning: the present invention will discard silastic product 450 DEG C of Thorough combustion 10min in Muffle furnace, and heating rate is 1-3 DEG C/min.By gained combustion product grind into powder, the powder diameter of formation is at about 500-1000nm.
(2) powder is shaping together with rubber: previous step gained powder screen cloth is sprinkled evenly tiling 0.5mm thickness forming mixing of rubber on the surface, the rubber sprinkled with powder is put into mould.
(3) hot-press vulcanization: in compression molding instrument, adopts the conditions of vulcanization of 150 DEG C and 14MPa, hot-press vulcanization 40min.
(4) demoulding post processing: mold takes out the rubber after hot-press vulcanization, is immersed in ethanol medium frequency 40Hz ultrasonic cleaning 10min, and surperficial by washed with de-ionized water.Wash away the powder not being pressed into surface, 40 DEG C of oven dry.One deck super hydrophobic surface can be formed on rubber surface surface.Whole operating process as shown in Figure 1.
The mixing of rubber formula of described forming is: rubber 100 parts, reinforced filling 100 parts, vulcanizing activator 12 parts, vulcanizing agent 5 parts, vulcanization accelerator 5 parts, vulcanization accelerator 5 parts, 25 parts, plasticizer, 6 parts, age resistor; By after above-mentioned mixing of materials first at 70 DEG C of 5min that plasticate, then after 110 DEG C of mixing 10min, namely obtain the mixing of rubber of forming.
Described rubber is butadiene rubber, butadiene-styrene rubber, natural rubber; Reinforced filling is N550; Vulcanizing activator is zinc oxide and stearic acid; Vulcanizing agent is sulphur and DCP; Vulcanization accelerator is thiazole accelerator DM or thuriam acceserator TMTD; Plasticizer is aromatic naphtha; Age resistor is antioxidant 4020 NA.
Embodiment 3
(1) the discarded silicon rubber of burning: the present invention will discard silastic product 600 DEG C of Thorough combustion 5min in Muffle furnace, and heating rate is 1-3 DEG C/min.By gained combustion product grind into powder, the powder diameter of formation is at about 200-500nm.
(2) powder is shaping together with rubber: previous step gained powder screen cloth is sprinkled evenly tiling 0.2mm thickness forming mixing of rubber on the surface, the rubber sprinkled with powder is put into mould.
(3) hot-press vulcanization: in compression molding instrument, adopts the conditions of vulcanization of 180 DEG C and 16MPa, hot-press vulcanization 30min.
(4) demoulding post processing: mold takes out the rubber after hot-press vulcanization, is immersed in ethanol medium frequency 50Hz ultrasonic cleaning 10min, and surperficial by washed with de-ionized water.Wash away the powder not being pressed into surface, 50 DEG C of oven dry.One deck super hydrophobic surface can be formed at rubber surface.Whole operating process as shown in Figure 1.
The mixing of rubber formula of described forming is: rubber 50 parts, reinforced filling 50 parts, vulcanizing activator 8 parts, vulcanizing agent 3 parts, vulcanization accelerator 3 parts, vulcanization accelerator 3 parts, 15 parts, plasticizer, 3 parts, age resistor; By after above-mentioned mixing of materials first at 50 DEG C of 8min that plasticate, then after 90 DEG C of mixing 13min, namely obtain the mixing of rubber of forming.
Described rubber is ethylene propylene diene rubber, butadiene rubber, butadiene-styrene rubber, one or more in natural rubber; Reinforced filling is one or more in N220, N234, N550; Vulcanizing activator is zinc oxide and/or stearic acid; Vulcanizing agent is sulphur and/or DCP; Vulcanization accelerator is one or more in sulfenamide type accelerators CZ, thiazole accelerator DM or thuriam acceserator TMTD; Plasticizer is one or more in coumarone indene resin, aromatic naphtha, carbon 5 Petropols, octyl group phenolic aldehyde BN-2; Age resistor is one or more in anti-aging agent RD, antioxidant 4020 NA, antioxidant MB.
Comparative example
The mixing of rubber identical with embodiment, in compression molding instrument, adopts the conditions of vulcanization of 150 DEG C and 14MPa, and hot-press vulcanization 40min obtains.Its surface topography as shown in Figure 2.
Above-mentioned use equipment is conventional production equipment.
Application Example 1 performance test
Laboratory surface wettability adopts Static Contact angle measuring instrument, tests embodiment 1-3 and comparative example's products obtained therefrom.To get three points on each surface and measure static contact angles, each point tolerance is no more than ± and 3 °, average.
Laboratory freezing performance test adopts horizontal thrust machine to test the shearing force of ice and rubber surface.Embodiment 1-3 and comparative example's products obtained therefrom are tested.The preparation method of sample is prepared into the sheet rubber of (6mm × 8mm × 2mm) according to rubber compounding sulfuration or is compounded with the sheet rubber of silicon rubber combustion powder super-hydrophobic layer.In the square plastic mould of (2.5mm × 2.5mm × 1.5mm), load 5ml distilled water then tip upside down on the rubbery sample of preparation.Constant temperature-20 DEG C ± 2 DEG C freezing 5h in refrigerator, be fixed on the adhesion values of the maximum ice of horizontal thrust machine experimental bench testing when ice and rubber surface depart from after taking-up immediately and characterize the power of adhesion between ice and specimen surface with this numerical value, measure three times under the same terms, get maximum.Experimental result is as table 1.
The surface wettability of table 1 comparative example of the present invention and embodiment and freezing performance comparison
| Performance test | Comparative example | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Contact angle (°) | 104±1 | 147±2 | 151±2 | 152±1 |
| The adhesion (N) of ice | 83.7 | 23.5 | 19 | 17.3 |
Can find out that the present invention greatly improves the static contact angle of rubber surface from upper table test result, reach super-hydrophobic rubber surface, this surface also has minimizing icing simultaneously, reduces the effect of icing adhesion.
After the present invention has constructed super hydrophobic surface on rubber, achieve automatically cleaning and freezing effect, be different from traditional clean and deicing mode.As shown in Figure 3 and Figure 4, static contact angle is 151 ° ± 2 for SEM (SEM) high power of prepared super hydrophobic surface and the image of low multiple.
Claims (4)
1. prepare a method for automatically cleaning freezing rubber surface with discarded silastic product, it is characterized in that step is as follows:
(1) burning of discarded silicon rubber: silastic product Thorough combustion will be discarded, then by gained combustion product grind into powder;
(2) shaping: obtained for step (1) powder to be laid in the mixing of rubber of forming on the surface, the rubber sprinkled with powder is put into mould;
(3) hot-press vulcanization: sulfidization molding in compression molding instrument;
(4) demoulding post processing: mold takes out the rubber after hot-press vulcanization, with ethanol and washed with de-ionized water surface, can form one deck super hydrophobic surface on rubber surface surface after oven dry.
2. prepare the method for automatically cleaning freezing rubber surface as claimed in claim 1 with discarded silastic product, it is characterized in that concrete steps are:
(1) burning of discarded silicon rubber: will discard silastic product in Muffle furnace at 300-600 DEG C Thorough combustion to burn 5-15min, heating rate is 1-3 DEG C/min; Then by gained combustion product grind into powder, described powder diameter is distributed between 100-1000nm;
(2) shaping: obtained for step (1) powder screen cloth is sprinkled evenly be laid in forming mixing of rubber on the surface, the thickness of powder bed is 0.2-1mm, then the rubber sprinkled with powder is put into mould;
(3) hot-press vulcanization: by step (2) gained material sulfidization molding in compression molding instrument; Curing temperature is 145-180 DEG C, and sulfide stress is 12-16MPa, the hot-press vulcanization time is 30-60min;
(4) demoulding post processing: mold takes out the rubber after hot-press vulcanization, and soak ultrasonic cleaning 5-10min in ethanol, supersonic frequency is 25-50Hz; Then use washed with de-ionized water surface, wash away the powder not being pressed into surface, 30-50 DEG C of oven dry, after oven dry, one deck super hydrophobic surface can be formed at rubber surface, namely obtain automatically cleaning freezing rubber surface.
3. the method for automatically cleaning freezing rubber surface is prepared as claimed in claim 2 with discarded silastic product, it is characterized in that: the mixing of rubber formula of described forming is: rubber 30-100 part, reinforced filling 0-100 part, vulcanizing activator 4-12 part, vulcanizing agent 0.2-5 part, vulcanization accelerator 0.8-5 part, vulcanization accelerator 0.8-5 part, plasticizer 5-25 part, age resistor 1-6 part; By after above-mentioned mixing of materials first at the 40-70 DEG C of 5-10min that plasticates, then after 70-110 DEG C of mixing 10-15min, namely obtain the mixing of rubber of forming.
4. prepare the method for automatically cleaning freezing rubber surface as claimed in claim 3 with discarded silastic product, it is characterized in that: described rubber is ethylene propylene diene rubber, butadiene rubber, butadiene-styrene rubber, one or more in natural rubber; Reinforced filling is one or more in N220, N234, N550; Vulcanizing activator is zinc oxide and/or stearic acid; Vulcanizing agent is sulphur and/or DCP; Vulcanization accelerator is one or more in sulfenamide type accelerators CZ, thiazole accelerator DM or thuriam acceserator TMTD; Plasticizer is one or more in coumarone indene resin, aromatic naphtha, carbon 5 Petropols, octyl group phenolic aldehyde BN-2; Age resistor is one or more in anti-aging agent RD, antioxidant 4020 NA, antioxidant MB.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109837758A (en) * | 2019-01-25 | 2019-06-04 | 河北科技大学 | A kind of preparation method of fabric super hydrophobic surface |
| CN110552079A (en) * | 2018-05-30 | 2019-12-10 | 中国石油化工股份有限公司 | Preparation method of super-hydrophobic polyester fiber |
| CN110551366A (en) * | 2018-05-30 | 2019-12-10 | 中国石油化工股份有限公司 | Preparation method of super-hydrophobic polyester film |
| CN112480468A (en) * | 2020-11-26 | 2021-03-12 | 杭州师范大学 | Method for preparing surface super-hydrophobic silicone rubber foam at ultra-fast speed and product thereof |
| CN113372836A (en) * | 2021-05-24 | 2021-09-10 | 三峡大学 | Preparation method of adhesive super-hydrophobic film |
| CN115008663A (en) * | 2022-04-28 | 2022-09-06 | 镇江同立橡胶有限公司 | One-time sintering vulcanization molding method and processing mold for rubber fender |
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| CN112480468B (en) * | 2020-11-26 | 2022-08-05 | 杭州师范大学 | Method for preparing surface super-hydrophobic silicone rubber foam at ultra-fast speed and product thereof |
| CN113372836A (en) * | 2021-05-24 | 2021-09-10 | 三峡大学 | Preparation method of adhesive super-hydrophobic film |
| CN115008663A (en) * | 2022-04-28 | 2022-09-06 | 镇江同立橡胶有限公司 | One-time sintering vulcanization molding method and processing mold for rubber fender |
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Application publication date: 20151230 |