CN105153819A - Method for preparing superhydrophobic coating by nano-crystalline cellulose template method - Google Patents
Method for preparing superhydrophobic coating by nano-crystalline cellulose template method Download PDFInfo
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Abstract
The invention provides a method for preparing a superhydrophobic coating by a nano-crystalline cellulose template method. Nano TiO2 with controllable particle diameter is generated on the surface of nano-crystalline cellulose in situ, the surface of nano TiO2 is subjected to hydrophobic modification through stearic acid, absolute ethyl alcohol is a solvent, and sodium dodecyl benzene sulfonate is a dispersant. TiO2 and PDMS (polydimethylsiloxane) which are modified by taking nano-crystalline cellulose (NCC) as the template are compounded and co-blended mechanically, and heat treatment is performed to obtain the superhydrophobic coating. The method has the advantages that as stearic acid serves as the modifier, and hydrophobic-CH3 group is introduced, the surface energy of TiO2/NCC is reduced; polydimethylsiloxane and TiO2/NCC are compounded, so that the adhesive force of the coating is improved, a micro/nano coarse structure is formed by interaction between TiO2/NCC and inorganic nano particles, and accordingly, the shortcoming of poor adhesion of TiO2/NCC is made up. The method is simple, the prepared coating can be widely added into various coatings to enhance the hydrophobicity, and the wearing resistance of a coating film can be guaranteed to a certain extent.
Description
Technical field
What the present invention relates to is the method for a kind of nano-crystalline cellulose template legal system for super-hydrophobic coat, belongs to coating and technical field of modification thereof.
Background technology
Aqueous coating compares traditional organic coating, has health, oligosaprobic feature.Meet the long-range road of Green Development, have broad application prospects.But there is the shortcoming such as water tolerance and poor mechanical property, invent a kind of novel super-hydrophobic coating and can well overcome this shortcoming.Patent CN104448960A discloses a kind of with stearic acid process TiO
2/ ZnO composite particles obtains the method for super-hydrophobic coat, by ZnO, TiO
2, ethanol, sodium laurylsulfonate and deionized water Homogeneous phase mixing, after normal temperature magnetic agitation 30min, obtained TiO
2/ ZnO composite particles; Then stearic acid is placed on ultrasonic abundant dissolving in dehydrated alcohol, finally by the stearic acid after dissolving and TiO
2/ ZnO composite particles mixes, 45-55 DEG C, the condition lower magnetic force of pH=3-5 stirs 6h, obtained modified hydrophobic coating.The method is simple take inorganic composite nanoparticles as modification basis, and the present invention take nano-cellulose as template and inductor, generates inorganic nano-particle TiO at its surface in situ
2, the micro-nano roughness causing hydrophobicity basic reason produces some superiority, and has followed the feature of nano-cellulose high strength and high tenacity, improve the mechanical property of coating.PDMS adds the surface energy also reducing coating, adds the bonding strength of coating.For the resultant performance enhancements of hydrophobic coating plays a positive role.
Summary of the invention
What the present invention proposed is the method for a kind of nano-crystalline cellulose template legal system for super-hydrophobic coat, and its object is intended to for the problem such as coating ubiquity water tolerance and poor mechanical property in the market, by the nano-TiO of nano-cellulose surface in situ generation size tunable
2, by stearic acid to making nano-TiO
2hydrophobically modified is carried out on surface, and dehydrated alcohol is solvent, and Sodium dodecylbenzene sulfonate is dispersion agent.The TiO that will be template modification with nano-cellulose (NCC)
2with PDMS (polydimethylsiloxane) compound, through mechanical blending, thermal treatment obtains super-hydrophobic coat.Make it possess self-cleaning function and to a certain extent improve coating abrasion performance and
The performances such as ductility.Preparation technology simply, does not need the instrument of complex and expensive to assist.
Technical solution of the present invention: by the method for nano-crystalline cellulose template legal system for super-hydrophobic coat, comprises the steps: to use nano-crystalline cellulose template legal system for the method for super-hydrophobic coat, comprises the steps:
1) with concentration 56% vitriolization Microcrystalline Cellulose MCC, part by weight MCC:H
2sO
4=1:(8.15-9.45) g/ml, acidolysis temperature is 45 DEG C, and the time is 90min-110min; Add deionized water and stop acidolysis reaction;
2) centrifuge washing is carried out, centrifugal speed 6000rpm, time 5min, number of times 3 times-4 times; Carry out dialysis subsequently and remove acid ion, 70% power ultrasonic process 20min-30min; Obtain nanofiber cellulose solution NCC, for subsequent use;
3) be V (TiCl by weight
4): the consumption of V (NCC)=1:10 is by TiCl
4slow instillation nanofiber cellulose solution, mechanical stirring 4h-5h at 70 DEG C;
4) distilled water, dehydrated alcohol, stearic acid is added, by adding TiCl
4quality 8%-8.5% counts, and stirs 2h, aging 2h-3h in air at 70 DEG C; Dry at 120 DEG C, grind out powder stand-by;
5) add deionized water, catalyst ammonia water and Sodium dodecylbenzene sulfonate, by drawing powder quality 1%, ultrasonic agitation 20-25min, to certain viscosity, adds powder, continues to stir 30min;
6) by V (TiCl
4): V (PDMS): V (KH550)=1:(0.5-1): the part by weight of (0.1-0.3), first slowly add PDMS, then add KH550, continue magnetic agitation, by solution coat in substrate surface, namely obtain super-hydrophobic coat.
Advantage of the present invention: using stearic acid as properties-correcting agent because its surface have a large amount of-COOH group exist, can with TiO
2there is dehydration reaction in the surface-OH of/NCC, and stearic acid also introduces hydrophobicity-CH
3group, thus reduce TiO
2the surface energy of/NCC; Polydimethylsiloxane (PDMS) has comparatively low surface energy and chemical stability, by itself and TiO
2/ NCC compound can effectively increase coating bonding strength, and by with the interaction of inorganic nano-particle formed micro-/receive coarse structure, compensate for TiO
2the shortcoming of/NCC poor adhesive force.Preparation method of the present invention is relatively simple, and extensively can add in multiple coating and strengthen its hydrophobic performance, and film wear resistance also has certain guarantee, has huge market practical value.
Accompanying drawing explanation
Fig. 1 is preparation flow figure of the present invention.
Embodiment
By the method for nano-crystalline cellulose template legal system for super-hydrophobic coat, comprise the steps:
1) with concentration 56% vitriolization Microcrystalline Cellulose MCC, part by weight MCC:H
2sO
4=1:(8.15-9.45) g/ml, acidolysis temperature is 45 DEG C, and the time is 90min-110min; Add deionized water and stop acidolysis reaction;
2) centrifuge washing is carried out, centrifugal speed 6000rpm, time 5min, number of times 3 times-4 times; Carry out dialysis subsequently and remove acid ion, 70% power ultrasonic process 20min-30min; Obtain nanofiber cellulose solution NCC, for subsequent use;
3) be V (TiCl by weight
4): the consumption of V (NCC)=1:10 is by TiCl
4slow instillation nanofiber cellulose solution, mechanical stirring 4h-5h at 70 DEG C;
4) distilled water, dehydrated alcohol, stearic acid is added, by adding TiCl
4quality 8%-8.5% counts, and stirs 2h, aging 2h-3h in air at 70 DEG C; Dry at 120 DEG C, grind out powder stand-by;
5) add deionized water, catalyst ammonia water and Sodium dodecylbenzene sulfonate, by drawing powder quality 1%, ultrasonic agitation 20-25min, to certain viscosity, adds powder, continues to stir 30min;
6) by V (TiCl
4): V (PDMS): V (KH550)=1:(0.5-1): the part by weight of (0.1-0.3), first slowly add PDMS, then add KH550, continue magnetic agitation, by solution coat in substrate surface, namely obtain super-hydrophobic coat.
The weight ratio that described step 1) adds deionized water termination reaction is H
2sO
4: H
2o=1:(2.5-3.5).
Described step 2) dialysis procedure is use the dialysis tubing of 8000-10000 molecular weight to dialyse, and changes 1 water every day, dialysis 3-4 days.
The each composition weight proportioning of described step 4) is, distilled water: dehydrated alcohol: stearic acid=50:(4.5-6.5): (0.5-1.5).
The each composition weight proportioning of described step 5) is, deionized water: ammoniacal liquor: Sodium dodecylbenzene sulfonate=(35-50): (0.5-1.5): 0.05.
It is 1.934mm that described step 5) ultrasonic agitation reaches certain viscosity
2/ s-2.132mm
2/ s.
After 45 DEG C of-55 DEG C of lower magnetic forces stir 1.5h-2.5h, add KH550 again after described step 6) adds PDMS, continue magnetic agitation 1h-2h.
Below in conjunction with specific embodiment, the invention will be further described;
Embodiment 1
By the method for nano-crystalline cellulose template legal system for super-hydrophobic coat, comprise the steps:
One, be that raw material sulphuric acid hydrolysis method prepares nanofiber cellulose solution with Microcrystalline Cellulose, concrete material amounts is than being MCC:H
2sO
4=1:8.45g/ml, 40 DEG C of reaction 95min in constant water bath box.Adding volume ratio is H
2sO
4: H
2the deionized water of O=1:2.5 stops acidolysis reaction.By sample with 6000r/m centrifugation 5min, remove supernatant liquor, centrifugal 3 times of repetitive operation, with 70% power ultrasonic process 20min.Obtain nanofiber cellulose solution (NCC); Two, by V (TiCl
4): the consumption of V (NCC)=1:10 is by TiCl
4slow instillation nanofiber cellulose solution, mechanical stirring 4h at 70 DEG C; Three, add be dissolved in ethanol stearic acid (by adding TiCl
4quality 8%), distilled water: dehydrated alcohol: stearic acid=50:4.5:0.8, stirs 2h at 70 DEG C, aging 2h in air.Dry at 120 DEG C, grind out powder (A) stand-by; Four, then add following component and mass ratio is deionized water: catalyst ammonia water: dispersion agent Sodium dodecylbenzene sulfonate=35:0.8:0.05, Sodium dodecylbenzene sulfonate (by drawing powder quality 1%), ultrasonic agitation 20min viscosity is to 1.998mm
2/ s, adds powders A, continues to stir 30min; Five, by V (TiCl
4): the ratio of V (PDMS): V (KH550)=1:0.8:0.3, first slowly adds PDMS and stirs 1.5h at 45 DEG C of lower magnetic forces, then add KH550, continue magnetic agitation 1.5h.
Finally after sheet glass complete for Best-Effort request at room temperature drying, 130 DEG C of bakings, until coating is fully solidified, obtain novel nano super hydrophobic composite coating.The static contact angle of compound coating of the present invention and water is 160.4 °, roll angle 5 °.
Embodiment 2
By the method for nano-crystalline cellulose template legal system for super-hydrophobic coat, comprise the steps:
One, be that raw material sulphuric acid hydrolysis method prepares nanofiber cellulose solution with Microcrystalline Cellulose, concrete material amounts is than being MCC:H
2sO
4=1:8.74g/ml, 40 DEG C of reaction 100min in constant water bath box.Adding volume ratio is H
2sO
4: H
2the deionized water of O=1:2.8 stops acidolysis reaction.By sample with 6000r/m centrifugation 5min, remove supernatant liquor, centrifugal 3 times of repetitive operation, with 70% power ultrasonic process 25min.Obtain nanofiber cellulose solution (NCC); Two, by V (TiCl
4): the consumption of V (NCC)=1:10 is by TiCl
4slow instillation nanofiber cellulose solution, mechanical stirring 4h at 70 DEG C; Three, add be dissolved in ethanol stearic acid (by adding TiCl
4quality 8.2%), distilled water: dehydrated alcohol: stearic acid=50:6:1.5, stirs 2h at 70 DEG C, aging 2.5h in air.Dry at 120 DEG C, grind out powder (A) stand-by; Four, then add following component and mass ratio is deionized water: catalyst ammonia water: dispersion agent Sodium dodecylbenzene sulfonate=40:1:0.05, Sodium dodecylbenzene sulfonate (by drawing powder quality 1%), ultrasonic agitation 20min viscosity is to 2.108mm
2/ s, adds powders A, continues to stir 30min; Five, by V (TiCl
4): the ratio of V (PDMS): V (KH550)=1:0.8:0.1, first slowly adds PDMS and stirs 1.5h at 45 DEG C of lower magnetic forces, then add KH550, continue magnetic agitation 1.5h.
Finally after sheet glass complete for Best-Effort request at room temperature drying, 130 DEG C of bakings, until coating is fully solidified, obtain novel nano super hydrophobic composite coating.The static contact angle of compound coating of the present invention and water is 152.5 °, roll angle 4 °.
Embodiment 3
By the method for nano-crystalline cellulose template legal system for super-hydrophobic coat, comprise the steps:
One, be that raw material sulphuric acid hydrolysis method prepares nanofiber cellulose solution with Microcrystalline Cellulose, concrete material amounts is than being MCC:H
2sO
4=1:9.3g/ml, 40 DEG C of reaction 98min in constant water bath box.Adding volume ratio is H
2sO
4: H
2the deionized water of O=1:3.2 stops acidolysis reaction.By sample with 6000r/m centrifugation 5min, remove supernatant liquor, centrifugal 4 times of repetitive operation, with 70% power ultrasonic process 28min.Obtain nanofiber cellulose solution (NCC); Two, by V (TiCl
4): the consumption of V (NCC)=1:10 is by TiCl
4slow instillation nanofiber cellulose solution, mechanical stirring 4h at 70 DEG C; Three, add be dissolved in ethanol stearic acid (by adding TiCl
4quality 8.2%), distilled water: dehydrated alcohol: stearic acid=50:6.5:0.7, stirs 2h at 70 DEG C, aging 2.5h in air.Dry at 120 DEG C, grind out powder (A) stand-by; Four, then add following component and mass ratio is deionized water: catalyst ammonia water: dispersion agent Sodium dodecylbenzene sulfonate=48:1.2:0.05, Sodium dodecylbenzene sulfonate (by drawing powder quality 1%), ultrasonic agitation 23min viscosity is to 2.015mm
2/ s, adds powders A, continues to stir 30min; Five, by V (TiCl
4): the ratio of V (PDMS): V (KH550)=1:0.7:0.15, first slowly adds PDMS and stirs 2h at 55 DEG C of lower magnetic forces, then add KH550, continue magnetic agitation 1.5h.
Finally after sheet glass complete for Best-Effort request at room temperature drying, 130 DEG C of bakings, until coating is fully solidified, obtain novel nano super hydrophobic composite coating.The static contact angle of compound coating of the present invention and water is 156.2 °, roll angle 5 °.
Claims (7)
1. use nano-crystalline cellulose template legal system for the method for super-hydrophobic coat, it is characterized in that comprising the steps:
1) with concentration 56% vitriolization Microcrystalline Cellulose MCC, part by weight MCC:H
2sO
4=1:(8.15-9.45) g/ml, acidolysis temperature is 45 DEG C, and the time is 90min-110min; Add deionized water and stop acidolysis reaction;
2) centrifuge washing is carried out, centrifugal speed 6000rpm, time 5min, number of times 3 times-4 times; Carry out dialysis subsequently and remove acid ion, 70% power ultrasonic process 20min-30min; Obtain nanofiber cellulose solution NCC, for subsequent use;
3) be V (TiCl by weight
4): the consumption of V (NCC)=1:10 is by TiCl
4slow instillation nanofiber cellulose solution, mechanical stirring 4h-5h at 70 DEG C;
4) distilled water, dehydrated alcohol, stearic acid is added, by adding TiCl
4quality 8%-8.5% counts, and stirs 2h, aging 2h-3h in air at 70 DEG C; Dry at 120 DEG C, grind out powder stand-by;
5) add deionized water, catalyst ammonia water and Sodium dodecylbenzene sulfonate, by drawing powder quality 1%, ultrasonic agitation 20-25min, to certain viscosity, adds powder, continues to stir 30min;
6) by V (TiCl
4): V (PDMS): V (KH550)=1:(0.5-1): the part by weight of (0.1-0.3), first slowly add PDMS, then add KH550, continue magnetic agitation, by solution coat in substrate surface, namely obtain super-hydrophobic coat.
2. nano-crystalline cellulose template legal system according to claim 1 is for the method for super-hydrophobic coat, it is characterized in that the weight ratio that described step 1) adds deionized water termination reaction is H
2sO
4: H
2o=1:(2.5-3.5).
3. nano-crystalline cellulose template legal system according to claim 1 is for the method for super-hydrophobic coat, it is characterized in that described step 2) dialysis procedure is use the dialysis tubing of 8000-10000 molecular weight to dialyse, and changes 1 water every day, dialysis 3-4 days.
4. nano-crystalline cellulose template legal system according to claim 1 is for the method for super-hydrophobic coat, it is characterized in that in each composition weight proportioning of described step 4) being, distilled water: dehydrated alcohol: stearic acid=50:(4.5-6.5): (0.5-1.5).
5. nano-crystalline cellulose template legal system according to claim 1 is for the method for super-hydrophobic coat, it is characterized in that each composition weight proportioning of described step 5) is, deionized water: ammoniacal liquor: Sodium dodecylbenzene sulfonate=(35-50): (0.5-1.5): 0.05.
6. nano-crystalline cellulose template legal system according to claim 1 is for the method for super-hydrophobic coat, and it is characterized in that described step 5) ultrasonic agitation reaches certain viscosity is 1.934mm
2/ s-2.132mm
2/ s.
7. the super-hydrophobic coat that nano-crystalline cellulose template legal system according to claim 1 is standby and method, is characterized in that described step 6) adds KH550 again after adding PDMS after 45 DEG C of-55 DEG C of lower magnetic forces stir 1.5h-2.5h, continue magnetic agitation 1h-2h.
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| CN114535022A (en) * | 2022-01-27 | 2022-05-27 | 中国石油大学(华东) | Preparation method of super-hydrophobic wear-resistant coating containing buffer structure |
| CN114535022B (en) * | 2022-01-27 | 2023-01-20 | 中国石油大学(华东) | Preparation method of super-hydrophobic wear-resistant coating containing buffer structure |
| CN117567938A (en) * | 2023-11-27 | 2024-02-20 | 河南城建学院 | Preparation method of water-based hydrophobic coating |
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Application publication date: 20151216 Assignee: Nanjing Dongfang Weiye Furniture Co., Ltd. Assignor: Nanjing Forestry University Contract record no.: 2019320000150 Denomination of invention: Method for preparing superhydrophobic coating by nano-crystalline cellulose template method Granted publication date: 20170531 License type: Common License Record date: 20190521 Application publication date: 20151216 Assignee: Nanjing DIO Furniture Co., Ltd. Assignor: Nanjing Forestry University Contract record no.: 2019320000151 Denomination of invention: Method for preparing superhydrophobic coating by nano-crystalline cellulose template method Granted publication date: 20170531 License type: Common License Record date: 20190521 |