CN105153819B - The method that super-hydrophobic coat is prepared with nano-crystalline cellulose template method - Google Patents
The method that super-hydrophobic coat is prepared with nano-crystalline cellulose template method Download PDFInfo
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Abstract
The present invention is a kind of method that nano-crystalline cellulose template method prepares super-hydrophobic coat, and the nano-TiO of size tunable is generated by nano-cellulose surface in situ2, by stearic acid to making nano-TiO2Surface carries out hydrophobically modified, and absolute ethyl alcohol is solvent, and neopelex is dispersant.Will be with nano-cellulose（NCC it is) TiO that template was modified2With PDMS (dimethyl silicone polymers）It is compound, through mechanical blending, it is thermally treated resulting in super-hydrophobic coat.Advantage：Using stearic acid as modifying agent, hydrophobicity CH is also introduced3Group, reduces TiO2The surface energy of/NCC；Dimethyl silicone polymer and TiO2/ NCC is compound to increase coating adhesive force, and by the interaction with inorganic nano-particle formed it is micro-/receive coarse structure, make up TiO2The shortcoming of/NCC poor adhesive forces.Method is simple, and can add extensively strengthen its hydrophobic performance in multiple coating, and film wearability also has certain guarantee.
Description
Technical field
The present invention relates to a kind of method that super-hydrophobic coat is prepared with nano-crystalline cellulose template method, belong to coating and its
Technical field of modification.
Background technology
Aqueous coating compare traditional organic coating, possess health, low stain the characteristics of.Meet the length of Green Development a long way
Road, has broad application prospects.But the shortcomings of there is water resistance and poor mechanical property, invents a kind of new super-hydrophobicity and applies
Layer can be very good to overcome this shortcoming.Patent CN104448960A discloses one kind with stearic acid treatment TiO2/ ZnO compound particles
The method for obtaining super-hydrophobic coat, by ZnO, TiO2, ethanol, dodecyl sodium sulfate and deionized water uniformly mix, normal temperature magnetic
After power stirring 30min, TiO is obtained2/ ZnO compound particles；Then ultrasound fully dissolves in stearic acid being placed on into absolute ethyl alcohol, most
Afterwards by the stearic acid and TiO after dissolving2/ ZnO compound particles mix, the magnetic agitation 6h under conditions of 45-55 DEG C, pH=3-5,
Modified hydrophobic coating is obtained.The method be it is simple be modified basis with inorganic composite nanoparticles, the present invention is with nanometer
Cellulose is template and derivant, in its surface in situ generation inorganic nano-particle TiO2, causing hydrophobicity basic reason
The characteristics of producing some superiority in micro-nano roughness, and followed nano-cellulose high intensity and high tenacity, improves coating
Mechanical property.The addition of PDMS also reduces the surface energy of coating, increased the adhesive force of coating.It is the synthesis of hydrophobic coating
Performance boost plays a positive role.
The content of the invention
Proposed by the present invention is a kind of method that nano-crystalline cellulose template method prepares super-hydrophobic coat, and its purpose is intended to pin
The problems such as to coating generally existing water resistance in the market and poor mechanical property, particle diameter is generated by nano-cellulose surface in situ
Controllable nano-TiO2, by stearic acid to making nano-TiO2Surface carries out hydrophobically modified, and absolute ethyl alcohol is solvent, dodecyl
Benzene sulfonic acid sodium salt is dispersant.Will be with nano-cellulose（NCC it is) TiO that template was modified2With PDMS (dimethyl silicone polymers）
It is compound, through mechanical blending, it is thermally treated resulting in super-hydrophobic coat.Make it possess self-cleaning function and improve to a certain extent to apply
Layer wearability and
The performances such as ductility.Preparation process is simple, the instrument auxiliary for not needing complex and expensive.
Technical solution of the invention：The method that super-hydrophobic coat is prepared with nano-crystalline cellulose template method, including it is as follows
Step：The method that super-hydrophobic coat is prepared with nano-crystalline cellulose template method, comprises the following steps：
1）With concentration 56% sulfuric acid treatment microcrystalline cellulose MCC, part by weight MCC:H2SO4=1：（8.15-9.45）G/ml,
Acidolysis temperature is 45 DEG C, and the time is 90min-110min；Deionized water is added to terminate acidolysis reaction；
2）Carry out centrifuge washing, centrifugal speed 6000rpm, time 5min, number of times 3 times -4 times；Then carry out dialysis removal
Acid ion, 70% power ultrasonic treatment 20min-30min；Nano-cellulose solution NCC, it is standby；
3）By weight it is V (TiCl4):V(NCC)=1:10 consumption is by TiCl4It is slowly dropped into nano-cellulose solution, 70
Mechanical agitation 4h-5h at DEG C；
4）Distilled water, absolute ethyl alcohol, stearic acid are added, by addition TiCl4Quality 8%-8.5% is counted, and 2h is stirred at 70 DEG C,
Aging 2h-3h in air；Dried at 120 DEG C, powder is ground stand-by；
5）Deionized water, catalyst ammonia water and neopelex are added, based on powder quality 1% is drawn, ultrasound
Stirring 20-25min adds powder to certain viscosity, continues to stir 30min；
6）By V (TiCl4):V(PDMS):V(KH550)=1:（0.5-1）:（0.1-0.3）Part by weight, it is first slow plus
Enter PDMS, be subsequently adding KH550, continue magnetic agitation, by solution coating in substrate surface, that is, obtain super-hydrophobic coat.
Advantages of the present invention：Using stearic acid as modifying agent, because there is substantial amounts of-COOH group to exist on its surface, can
With with TiO2There is dehydration in the surface-OH of/NCC, and stearic acid also introduces hydrophobicity-CH3Group, so as to reduce
TiO2The surface energy of/NCC；Dimethyl silicone polymer（PDMS) have compared with low-surface-energy and chemical stability, by itself and TiO2/NCC
It is compound to be effectively increased coating adhesive force, and by the interaction with inorganic nano-particle formed it is micro-/receive coarse structure, more
TiO is mended2The shortcoming of/NCC poor adhesive forces.Preparation method of the invention is relatively easy, and can extensively add multiple coating
Middle its hydrophobic performance of enhancing, film wearability also has certain guarantee, possesses huge market practical value.
Brief description of the drawings
Fig. 1 is preparation flow figure of the invention.
Specific embodiment
The method that super-hydrophobic coat is prepared with nano-crystalline cellulose template method, comprises the following steps：
1）With concentration 56% sulfuric acid treatment microcrystalline cellulose MCC, part by weight MCC:H2SO4=1：（8.15-9.45）G/ml,
Acidolysis temperature is 45 DEG C, and the time is 90min-110min；Deionized water is added to terminate acidolysis reaction；
2）Carry out centrifuge washing, centrifugal speed 6000rpm, time 5min, number of times 3 times -4 times；Then carry out dialysis removal
Acid ion, 70% power ultrasonic treatment 20min-30min；Nano-cellulose solution NCC, it is standby；
3）By weight it is V (TiCl4):V(NCC)=1:10 consumption is by TiCl4It is slowly dropped into nano-cellulose solution, 70
Mechanical agitation 4h-5h at DEG C；
4）Distilled water, absolute ethyl alcohol, stearic acid are added, by addition TiCl4Quality 8%-8.5% is counted, and 2h is stirred at 70 DEG C,
Aging 2h-3h in air；Dried at 120 DEG C, powder is ground stand-by；
5）Deionized water, catalyst ammonia water and neopelex are added, based on powder quality 1% is drawn, ultrasound
Stirring 20-25min adds powder to certain viscosity, continues to stir 30min；
6）By V (TiCl4):V(PDMS):V(KH550)=1:（0.5-1）:（0.1-0.3）Part by weight, it is first slow plus
Enter PDMS, be subsequently adding KH550, continue magnetic agitation, by solution coating in substrate surface, that is, obtain super-hydrophobic coat.
The step 1）The weight ratio for adding deionized water terminating reaction is H2SO4:H2O=1:(2.5-3.5)。
The step 2）Dialysis procedure is to be dialysed using the bag filter of 8000-10000 molecular weight, and 1 water is changed daily,
Dialysis 3-4 days.
The step 4）Each component weight proportion is, distilled water：Absolute ethyl alcohol：Stearic acid=50：（4.5-6.5）：（0.5-
1.5）.
The step 5）Each component weight proportion is, deionized water：Ammoniacal liquor：Neopelex=（35-50）：
（0.5-1.5）：0.05.
The step 5）Ultrasonic agitation reaches certain viscosity for 1.934mm2/s-2.132mm2/s。
The step 6）KH550 is added after magnetic agitation 1.5h-2.5h at 45 DEG C -55 DEG C after adding PDMS, is continued
Magnetic agitation 1h-2h.
Below in conjunction with specific embodiment, the invention will be further described；
Embodiment 1
The method that super-hydrophobic coat is prepared with nano-crystalline cellulose template method, comprises the following steps：
First, nano-cellulose solution is prepared by raw material sulphuric acid Hydrolyze method of microcrystalline cellulose, specific material amounts ratio is
MCC:H2SO4=1：8.45g/ml, 40 DEG C of reaction 95min in constant water bath box.Addition volume ratio is H2SO4:H2O=1:2.5
Deionized water terminates acidolysis reaction.By sample with 6000r/m centrifugation 5min, supernatant is removed, repeats centrifugation 3 times,
20min is processed with 70% power ultrasonic.Obtain nano-cellulose solution (NCC)；2nd, by V (TiCl4):V(NCC)=1:10 consumption
By TiCl4Nano-cellulose solution is slowly dropped into, mechanical agitation 4h at 70 DEG C；3rd, the stearic acid for being dissolved in ethanol is added（By addition
TiCl4Quality 8% is counted）, distilled water：Absolute ethyl alcohol：Stearic acid=50：4.5：2h is stirred at 0.8,70 DEG C, aging 2h in air.
Dried at 120 DEG C, powder is ground（A it is) stand-by；4th, it is subsequently adding following component and mass ratio is deionized water：Catalysis
Agent ammoniacal liquor：Dispersant neopelex=35：0.8：0.05, neopelex（By drawing powder quality 1%
Meter）, ultrasonic agitation 20min viscositys to 1.998mm2/ s, adds powders A, continues to stir 30min；5th, by V (TiCl4):V
(PDMS):V(KH550)=1:0.8:0.3 ratio, is first slowly added to PDMS magnetic agitation 1.5h at 45 DEG C, is subsequently adding
KH550, continues magnetic agitation 1.5h.
After finally the sheet glass that Best-Effort request is finished is dried at room temperature for, 130 DEG C of bakings fully solidify until coating, make
Obtain novel nano super hydrophobic composite coating.Composite coating of the invention is 160.4 °, 5 ° of roll angle with the static contact angle of water.
Embodiment 2
The method that super-hydrophobic coat is prepared with nano-crystalline cellulose template method, comprises the following steps：
First, nano-cellulose solution is prepared by raw material sulphuric acid Hydrolyze method of microcrystalline cellulose, specific material amounts ratio is
MCC:H2SO4=1：8.74g/ml, 40 DEG C of reaction 100min in constant water bath box.Addition volume ratio is H2SO4:H2O=1:2.8
Deionized water terminates acidolysis reaction.By sample with 6000r/m centrifugation 5min, supernatant is removed, repeats centrifugation 3 times,
25min is processed with 70% power ultrasonic.Obtain nano-cellulose solution (NCC)；2nd, by V (TiCl4):V(NCC)=1:10 consumption
By TiCl4Nano-cellulose solution is slowly dropped into, mechanical agitation 4h at 70 DEG C；3rd, the stearic acid for being dissolved in ethanol is added（By addition
TiCl4Quality 8.2% is counted）, distilled water：Absolute ethyl alcohol：Stearic acid=50：6：2h is stirred at 1.5,70 DEG C, it is aging in air
2.5h.Dried at 120 DEG C, powder is ground（A it is) stand-by；4th, it is subsequently adding following component and mass ratio is deionized water：
Catalyst ammonia water：Dispersant neopelex=40：1：0.05, neopelex（By drawing powder quality
1% meter）, ultrasonic agitation 20min viscositys to 2.108mm2/ s, adds powders A, continues to stir 30min；5th, by V (TiCl4):V
(PDMS):V(KH550)=1:0.8:0.1 ratio, is first slowly added to PDMS magnetic agitation 1.5h at 45 DEG C, is subsequently adding
KH550, continues magnetic agitation 1.5h.
After finally the sheet glass that Best-Effort request is finished is dried at room temperature for, 130 DEG C of bakings fully solidify until coating, make
Obtain novel nano super hydrophobic composite coating.Composite coating of the invention is 152.5 °, 4 ° of roll angle with the static contact angle of water.
Embodiment 3
The method that super-hydrophobic coat is prepared with nano-crystalline cellulose template method, comprises the following steps：
First, nano-cellulose solution is prepared by raw material sulphuric acid Hydrolyze method of microcrystalline cellulose, specific material amounts ratio is
MCC:H2SO4=1：9.3g/ml, 40 DEG C of reaction 98min in constant water bath box.Addition volume ratio is H2SO4:H2O=1:3.2 go
Ionized water terminates acidolysis reaction.By sample with 6000r/m centrifugation 5min, supernatant is removed, repeat centrifugation 4 times, with
70% power ultrasonic processes 28min.Obtain nano-cellulose solution (NCC)；2nd, by V (TiCl4):V(NCC)=1:10 consumption will
TiCl4Nano-cellulose solution is slowly dropped into, mechanical agitation 4h at 70 DEG C；3rd, the stearic acid for being dissolved in ethanol is added（By addition
TiCl4Quality 8.2% is counted）, distilled water：Absolute ethyl alcohol：Stearic acid=50：6.5：2h is stirred at 0.7,70 DEG C, it is aging in air
2.5h.Dried at 120 DEG C, powder is ground（A it is) stand-by；4th, it is subsequently adding following component and mass ratio is deionized water：
Catalyst ammonia water：Dispersant neopelex=48：1.2：0.05, neopelex（By drawing powder quality
1% meter）, ultrasonic agitation 23min viscositys to 2.015mm2/ s, adds powders A, continues to stir 30min；5th, by V (TiCl4):V
(PDMS):V(KH550)=1:0.7:0.15 ratio, is first slowly added to PDMS magnetic agitation 2h at 55 DEG C, is subsequently adding
KH550, continues magnetic agitation 1.5h.
After finally the sheet glass that Best-Effort request is finished is dried at room temperature for, 130 DEG C of bakings fully solidify until coating, make
Obtain novel nano super hydrophobic composite coating.Composite coating of the invention is 156.2 °, 5 ° of roll angle with the static contact angle of water.
Claims (1)
1. the method that super-hydrophobic coat is prepared with nano-crystalline cellulose template method, it is characterised in that comprise the following steps：
1）With concentration 56% sulfuric acid treatment microcrystalline cellulose MCC, part by weight MCC：H2SO4=1：(8.15-9.45), acidolysis temperature
It is 45 DEG C to spend, and the time is 90min-110min；Deionized water is added to terminate acidolysis reaction；
2）Carry out centrifuge washing, centrifugal speed 6000rpm, time 5min, number of times 3 times -4 times；Then carry out dialysis removal acid group
Ion, 70% power ultrasonic treatment 20min-30min；Nano-cellulose solution NCC, it is standby；
3）It is by volume V (TiCl4) ：V（NCC）=1：10 consumption is by TiCl4It is slowly dropped into nano-cellulose solution, 70 DEG C
Lower mechanical agitation 4h-5h；
4）Distilled water, absolute ethyl alcohol, stearic acid are added, by addition TiCl4Quality 8%-8.5% is counted, and 2h, air are stirred at 70 DEG C
In aging 2h-3h；Dried at 120 DEG C, powder is ground stand-by；
5）Add deionized water, catalyst ammonia water and neopelex, based on powder quality 1% is drawn, ultrasonic agitation
20-25min adds powder to certain viscosity, continues to stir 30min；
6）By V (TiCl4):V(PDMS):V(KH550)=1:（0.5-1）:（0.1-0.3）Volume ratio, be first slowly added to
PDMS, is subsequently adding KH550, continues magnetic agitation, by solution coating in substrate surface, that is, obtains super-hydrophobic coat；
The step 1）The weight ratio for adding deionized water terminating reaction is H2SO4:H2O=1:(2.5-3.5)；
The step 2）Dialysis procedure is to be dialysed using the bag filter of 8000-10000 molecular weight, and 1 water is changed daily, dialysis
3-4 days；
The step 4）Each component weight proportion is, distilled water：Absolute ethyl alcohol：Stearic acid=50：（4.5-6.5）：（0.5-1.5）；
The step 5）Each component weight proportion is, deionized water：Ammoniacal liquor：Neopelex=（35-50）：（0.5-
1.5）：0.05；
The step 5）Ultrasonic agitation reaches certain viscosity for 1.934mm2/s-2.132mm2/s；
The step 6）KH550 is added after magnetic agitation 1.5h-2.5h at 45 DEG C -55 DEG C after adding PDMS, continues magnetic force
Stirring 1h-2h.
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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 |
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