CN108911525A - A kind of preparation method of hydrophobic core material - Google Patents
A kind of preparation method of hydrophobic core material Download PDFInfo
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- CN108911525A CN108911525A CN201810878474.4A CN201810878474A CN108911525A CN 108911525 A CN108911525 A CN 108911525A CN 201810878474 A CN201810878474 A CN 201810878474A CN 108911525 A CN108911525 A CN 108911525A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
- C03C17/30—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
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Abstract
The invention discloses a kind of preparation methods of hydrophobic core material, belong to hydrophobic material preparation technical field.The method of the present invention is that core material is exposed under organosilane reagents atmosphere, so that organosilane reagents and the hydroxyl condensation on core material surface is formed hydrophobic silane coating, specifically includes following steps：Organic-silylation reagent is added into container, then will be placed in container with core material, closed container heats it, comes into full contact with the gasification of organic-silylation reagent with core material and reacts, obtains hydrophobic core material.The method of the present invention simple process, non-environmental-pollution is at low cost, and the hydrophobically modified sand core funnel obtained according to the method for the present invention, hydrophobicity is good, can be used for the fields such as wastewater treatment, water-oil separating, lotion separation, has good industrial applications prospect.
Description
Technical field
The invention belongs to hydrophobic material preparation technical fields, and in particular to a kind of preparation method of hydrophobic core material.
Background technique
The sand core filter plate of sand core funnel is to use the high boron of excellent hard by being sieved and then being sintered after frits
Glass composition, physicochemical property with higher can filter acid solution and be handled with acids, also be acid funnel, the leakage of glass incipient fusion
Bucket.Sand core funnel is a kind of filter device that may be implemented to be separated by solid-liquid separation, and has many advantages, such as simple, quick, at low cost, extensive use
In chemical analysis, the monitoring of hygiene, environmental monitoring, biological products, scientific research etc..The sand core filter plate master of usual sand core funnel
Wanting ingredient is silica, and great amount of hydroxy group is contained on surface, high energy, water-wetted surface is formed, when being filtered to differences such as water, oil
Solvent is without selectivity.For the practical application for expanding sand core funnel, sand core filter plate needs to carry out hydrophobically modified, reaches good oil
Water separating effect.For prepare have special wetability material frequently with method include biomimetic method, chemical modification, layer by layer from
Assembling, template, chemical etching method, spray coating method and czochralski method etc..Specifically have and is drawn by surface grafting, click-reaction and copper
The active free radical polymerization of hair, by modified glass surface water contact angle reach 90 ° or more (Polym.Chem., 2017,
8,7457–7468).The silica nanosphere that trimethyl silicone hydride is synthesized by sol-gel method, with silica net
It is formed on network surface based superhydrophobic thin films (ACS Appl.Mater.Interfaces, 2011,3,3440-3447).Pass through immersion method
By silicon wafer infiltration in the mixed solution of silane coupling agent and organic solvent, post-processed using cleaning, dry etc. are a series of
Journey obtains super hydrophobic surface (J.Am.Chem.Soc., 2006,128,9052-9053).It will be mesoporous by LBL self-assembly method
Silicon dioxide granule is assembled into the coating of hierarchical structure, the glass surface that obtains there is superhydrophobic property (Langmuir, 2010,
26,13528–13534).Preparing hydrophobic surface in silica surface, presently, there are following technological difficulties：It is existing prepare it is hydrophobic
Property silica based materials method and steps it is complicated, previous materials building is complicated and aftertreatment technology is relatively complicated, production cost
It is higher, large-scale application possibility very little.Importantly, sand core filter plate has inherent advantage, it is by different size of gravel group
At the pore size distribution range of formation is wide, arrives several hundred thousands of microns greatly, as low as less than 1 micron, constitutes the table with different roughness
Face can satisfy the demand of all kinds of oil mixing with water separation after hydrophobically modified.Develop a kind of simple, low cost and have and answers
It is extremely urgent with the hydrophobic core material of value.
Summary of the invention
In order to overcome problems of the prior art, the purpose of the present invention is to provide a kind of systems of hydrophobic core material
Preparation Method, this method are chemical vapour deposition technique, and hydrophobic core material, technique can be prepared using single step reaction in situ
Simply, non-environmental-pollution, at low cost.The object of the invention is also to provide the applications of prepared hydrophobic core material.
The purpose of the invention is achieved by the following technical solution：
A kind of preparation method of hydrophobic core material makes to have for core material to be exposed under organosilane reagents atmosphere
Machine silane reagent and the hydroxyl condensation on core material surface form hydrophobic silane coating, obtain hydrophobic core material.Wherein, institute
The organosilane reagents atmosphere stated is by being vaporized to obtain to organosilane reagents heating.The core material includes sand
Core funnel, sand core piece etc..
Preferably, the organosilane reagents include hexamethyldisilazane, methyltrimethoxysilane, dodecyl
Trimethoxy silane, perfluoro capryl triethoxysilane, octadecyl trichlorosilane alkane etc..It is further preferred that described is organic
Silane reagent is perfluoro capryl triethoxysilane.
More specifically, the preparation method of the hydrophobic core material, includes the following steps：Organosilicon is added into container
Alkylators and core material (core material is not contacted with organic-silylation reagent), closed container heats container, makes
The gasification of organic-silylation reagent comes into full contact with core material, obtains hydrophobic core material.Preferably, before being heated to container
It is vacuumized, the temperature of heating is 40~140 DEG C, and the time of heating is 10min~for 24 hours.
A kind of hydrophobic core material, is obtained by above-mentioned preparation method.
The hydrophobic core material can be using fields such as water-oil separating, lotion separation, wastewater treatments.
The principle of the present invention：The main component of core material is silica, surface silicone hydroxyl rich in, Ke Yifa
A series of raw derivative reactions related with hydroxyl make organosilane reagents gasify, core material are completely exposed by heating
It under silane reagent atmosphere, comes into full contact with, forms hydrophobic silane coating with the hydroxyl condensation of the surface of solids, and then construct sand core
The hydrophobic surface of material.
The present invention has the following technical effect that：
(1) the method for the present invention simple process, non-environmental-pollution are not necessarily to any expensive device.
(2) the hydrophobically modified sand core funnel obtained according to the method for the present invention, hydrophobicity is good, water contact angle can reach 90 °~
150 °, it is resistant to acid-base salt solution, it is at low cost, it can be used for the fields such as wastewater treatment, water-oil separating, lotion separation, have good
Industrial applications prospect.
Detailed description of the invention
Fig. 1 is type dryer used and to prepare the schematic diagram of hydrophobically modified sand core funnel in the embodiment of the present invention.
Fig. 2 is the water contact angle knot of sand core funnel (a) and modified sand core funnel (b) before modified in the embodiment of the present invention 1
Fruit figure.
Fig. 3 is the water contact angle result of the embodiment of the present invention 2 sand core funnel (a) and modified sand core funnel (b) before modified
Figure.
Fig. 4 be the embodiment of the present invention 2 in modified sand core funnel separation of methylbenzene/water mixed liquid result figure (a) and chloroform/
The result figure (b) of water mixed liquid.
Fig. 5 is the modified sand core funnel of the embodiment of the present invention 2 to pH=1 sulfuric acid solution (a), pH=13 sodium hydroxide solution
(b) and the water contact angle result figure of 5wt% sodium chloride solution (c).
Fig. 6 is the water contact angle result figure that the present invention applies example 3 sand core funnel (a) and modified sand core funnel (b) before modified.
Fig. 7 is the water contact angle result that the present invention implements 4 sand core funnels (a) and modified sand core funnel (b) before modified
Figure.
Fig. 8 is the water contact angle result of the embodiment of the present invention 5 sand core funnel (a) and modified sand core funnel (b) before modified
Figure.
Fig. 9 is the water contact angle result of the embodiment of the present invention 6 sand core funnel (a) and modified sand core funnel (b) before modified
Figure.
Figure 10 is the water contact angle result of the embodiment of the present invention 7 sand core funnel (a) and modified sand core funnel (b) before modified
Figure.
Figure 11 is the water contact angle result of the embodiment of the present invention 8 sand core funnel (a) and modified sand core funnel (b) before modified
Figure.
Figure 12 is the water contact angle result of the embodiment of the present invention 9 sand core funnel (a) and modified sand core funnel (b) before modified
Figure.
Figure 13 is the water contact angle knot of the embodiment of the present invention 10 sand core funnel (a) and modified sand core funnel (b) before modified
Fruit figure.
Figure 14 is the water contact angle knot of the embodiment of the present invention 14 sand core funnel (a) and modified sand core funnel (b) before modified
Fruit figure.
Specific embodiment
Further detailed description is done to the present invention below with reference to embodiment, it should be appreciated that provided embodiment is only pair
The explanation of the method for the present invention, remaining content without limiting the invention in any way announcement.
【Embodiment 1】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G1 is placed in drier, is placed in drier bottom
One small incubation ware, as shown in Figure 1,10mL perfluoro capryl triethoxysilane is wherein added, by drier vacuum state,
It is put into 140 DEG C of baking ovens to heat 4 hours, taking-up, which is cooled to room temperature, obtains hydrophobically modified sand core funnel, and water/air contact angle is
131 °, the contact angle of rear sand core funnel is substantially change before modified as can be seen from Figure 2, by the above method, is successfully dredged
Water is modified sand core funnel, reaches excellent hydrophobic effect.
【Embodiment 2】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G2 is placed in drier, is placed in drier bottom
One small incubation ware, as shown in Figure 1,10mL perfluoro capryl triethoxysilane is wherein added, by drier vacuum state,
It is put into 140 DEG C of baking ovens to heat 4 hours, taking-up, which is cooled to room temperature, obtains hydrophobically modified sand core funnel, and water/air contact angle is
136 °, the contact angle of rear sand core funnel is substantially change before modified as can be seen from Figure 3, by the above method, is successfully dredged
Water is modified sand core funnel, reaches excellent hydrophobic effect.Modified sand core funnel is used for water-oil separating, Fig. 4 shows modification
G2 funnel separates toluene/water, chloroform/water mixed liquor separation figure, oil-water mixture success afterwards, and organic solvent all passes through and changes
Property after G2 funnel, and water remains entirely in above, and entire separation process is completed in more than ten seconds, and separating rate is fast and separating effect
It is excellent.Fig. 5 shows modified sand core funnel G2 to the water contact angle of acid-alkali salt, wherein to the sulfuric acid solution water contact angle of pH=1
It is 129 °, the sodium hydroxide solution water contact angle to pH=13 is 125 °, and the sodium chloride solution water contact angle to 5wt% is
129 °, show excellent acid and alkali-resistance effect.
【Embodiment 3】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G3 is placed in drier, is placed in drier bottom
One small incubation ware, as shown in Figure 1,10mL perfluoro capryl triethoxysilane is wherein added, by drier vacuum state,
It is put into 140 DEG C of baking ovens to heat 4 hours, taking-up, which is cooled to room temperature, obtains hydrophobically modified sand core funnel, and water/air contact angle is
140 °, the contact angle of rear sand core funnel is substantially change before modified as can be seen from Figure 6, by the above method, is successfully dredged
Water is modified sand core funnel, reaches excellent hydrophobic effect.
【Embodiment 4】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G4 is placed in drier, is placed in drier bottom
One small incubation ware, as shown in Figure 1,10mL perfluoro capryl triethoxysilane is wherein added, by drier vacuum state,
It is put into 140 DEG C of baking ovens to heat 4 hours, taking-up, which is cooled to room temperature, obtains hydrophobically modified sand core funnel, and water/air contact angle is
145 °, the contact angle of rear sand core funnel is substantially change before modified as can be seen from Figure 7, by the above method, is successfully dredged
Water is modified sand core funnel, reaches excellent hydrophobic effect.
【Embodiment 5】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G5 is placed in drier, is placed in drier bottom
One small incubation ware, as shown in Figure 1,10mL perfluoro capryl triethoxysilane is wherein added, by drier vacuum state,
It is put into 140 DEG C of baking ovens to heat 4 hours, taking-up, which is cooled to room temperature, obtains hydrophobically modified glass, and water/air contact angle is
147 °, the contact angle of rear sand core funnel is substantially change before modified as can be seen from Figure 8, by the above method, is successfully dredged
Water is modified sand core funnel, reaches excellent hydrophobic effect.
【Embodiment 6】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G6 is placed in drier, is placed in drier bottom
One small incubation ware, as shown in Figure 1,10mL perfluoro capryl triethoxysilane is wherein added, by drier vacuum state,
It is put into 140 DEG C of baking ovens to heat 4 hours, taking-up, which is cooled to room temperature, obtains hydrophobically modified sand core funnel, and water/air contact angle is
150 °, the contact angle of rear sand core funnel is substantially change before modified as can be seen from Figure 9, by the above method, is successfully dredged
Water is modified sand core funnel, reaches excellent hydrophobic effect.
【Embodiment 7】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G6 is placed in drier, is placed in drier bottom
Drier vacuum state is put by one small incubation ware as shown in Figure 1,10mL hexamethyldisilazane is wherein added
140 DEG C of baking ovens heat 4 hours, and taking-up, which is cooled to room temperature, obtains hydrophobically modified sand core funnel, and water/air contact angle is
143 °, the contact angle of rear sand core funnel is substantially change before modified as can be seen from Figure 10, by the above method, is successfully dredged
Water is modified sand core funnel, reaches excellent hydrophobic effect.
【Embodiment 8】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G6 is placed in drier, is placed in drier bottom
Drier vacuum state is put by one small incubation ware as shown in Figure 1,10mL methyltrimethoxysilane is wherein added
140 DEG C of baking ovens heat 4 hours, and taking-up, which is cooled to room temperature, obtains hydrophobically modified sand core funnel, and water/air contact angle is
138 °, the contact angle of rear sand core funnel is substantially change before modified as can be seen from Figure 11, by the above method, is successfully dredged
Water is modified sand core funnel, reaches excellent hydrophobic effect.
【Embodiment 9】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G6 is placed in drier, is placed in drier bottom
One small incubation ware, as shown in Figure 1,10mL dodecyltrimethoxysilane is wherein added, by drier vacuum state,
It is put into 140 DEG C of baking ovens to heat 4 hours, taking-up, which is cooled to room temperature, obtains hydrophobically modified sand core funnel, and water/air contact angle is
141 °, the contact angle of rear sand core funnel is substantially change before modified as can be seen from Figure 12, by the above method, is successfully dredged
Water is modified sand core funnel, reaches excellent hydrophobic effect.
【Embodiment 10】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G6 is placed in drier, is placed in drier bottom
Drier vacuum state is put by one small incubation ware as shown in Figure 1,10mL octadecyl trichlorosilane alkane is wherein added
140 DEG C of baking ovens heat 10min, and taking-up, which is cooled to room temperature, obtains hydrophobically modified sand core funnel, and water/air contact angle is
141 °, the contact angle of rear sand core funnel is substantially change before modified as can be seen from Figure 13, by the above method, is successfully dredged
Water is modified sand core funnel, reaches excellent hydrophobic effect.
【Embodiment 11】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G6 is placed in drier, is placed in drier bottom
One small incubation ware, as shown in Figure 1,10mL perfluoro capryl triethoxysilane is wherein added, by drier vacuum state,
40 DEG C of baking oven heating 30min are put into, taking-up, which is cooled to room temperature, obtains hydrophobically modified sand core funnel, and water/air contact angle is
124°。
【Embodiment 12】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G6 is placed in drier, is placed in drier bottom
One small incubation ware, as shown in Figure 1,10mL perfluoro capryl triethoxysilane is wherein added, by drier vacuum state,
70 DEG C of baking oven heating 30min are put into, taking-up, which is cooled to room temperature, obtains hydrophobically modified sand core funnel, and water/air contact angle is
134°。
【Embodiment 13】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G6 is placed in drier, is placed in drier bottom
It is small to be put into 70 DEG C of baking oven heating 24 as shown in Figure 1,10mL perfluoro capryl triethoxysilane is wherein added for one small incubation ware
When, taking-up, which is cooled to room temperature, obtains hydrophobically modified sand core funnel, and water/air contact angle is 145 °.
【Embodiment 14】
Firstly, being cleaned by ultrasonic the time every time is 5 minutes with alternately ultrasonic cleaning sand core funnel 3 times of dehydrated alcohol and acetone,
It is cleaned 3 times with deionized water again, then uses hot blast drying.Sand core funnel G6 is placed in drier, is placed in drier bottom
It is small to be put into 140 DEG C of baking oven heating 4 as shown in Figure 1,10mL perfluoro capryl triethoxysilane is wherein added for one small incubation ware
When, taking-up, which is cooled to room temperature, obtains hydrophobically modified sand core funnel, and water/air contact angle is 144 °, as can be seen from Figure 14
The contact angle of sand core funnel is substantially change after before modified, by the above method, has successfully been obtained hydrophobically modified sand core funnel, has been reached
Excellent hydrophobic effect.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of hydrophobic core material, it is characterised in that：The preparation method is to be exposed to core material
Under organosilane reagents atmosphere, organosilane reagents and the hydroxyl condensation on core material surface is made to form hydrophobic silane coating,
Obtain hydrophobic core material.
2. preparation method according to claim 1, it is characterised in that：The organosilane reagents atmosphere is by having
The heating of machine silane reagent is vaporized to obtain.
3. preparation method according to claim 1, it is characterised in that：The core material includes sand core funnel, sand core
Piece.
4. preparation method according to claim 1, it is characterised in that：The organosilane reagents include two silicon of hexamethyl
Azane, methyltrimethoxysilane, dodecyltrimethoxysilane, perfluoro capryl triethoxysilane, octadecyl trichlorine
Silane.
5. the preparation method according to claim 4, it is characterised in that：The organosilane reagents are three second of perfluoro capryl
Oxysilane.
6. preparation method according to claim 1, it is characterised in that：Include the following steps：Organosilicon is added into container
Alkylators and core material, closed container heat container, keep the gasification of organic-silylation reagent abundant with core material
Contact, obtains hydrophobic core material.
7. preparation method according to claim 6, it is characterised in that：It is vacuumized before being heated to container.
8. preparation method according to claim 6, it is characterised in that：The temperature of heating is 40~140 DEG C, the time of heating
For 10min~for 24 hours.
9. a kind of hydrophobic core material, it is characterised in that：It is obtained by the described in any item preparation methods of claim 1-8.
10. application of the hydrophobic core material as claimed in claim 9 in water-oil separating, lotion separation or field of waste water treatment.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110560017A (en) * | 2019-08-14 | 2019-12-13 | 上海应用技术大学 | Preparation method of alkylation modified silica gel |
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|---|---|---|---|---|
| WO2017058969A1 (en) * | 2015-10-02 | 2017-04-06 | Corning Incorporated | Removable glass surface treatments and methods for reducing particle adhesion |
| CN107365423A (en) * | 2017-08-07 | 2017-11-21 | 武汉大学 | A kind of hydrophobically modified method of cellulose |
| CN107383212A (en) * | 2017-08-07 | 2017-11-24 | 武汉大学 | A kind of hydrophobically modified method of nano-cellulose |
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2018
- 2018-08-03 CN CN201810878474.4A patent/CN108911525B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017058969A1 (en) * | 2015-10-02 | 2017-04-06 | Corning Incorporated | Removable glass surface treatments and methods for reducing particle adhesion |
| CN107365423A (en) * | 2017-08-07 | 2017-11-21 | 武汉大学 | A kind of hydrophobically modified method of cellulose |
| CN107383212A (en) * | 2017-08-07 | 2017-11-24 | 武汉大学 | A kind of hydrophobically modified method of nano-cellulose |
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| CN110560017A (en) * | 2019-08-14 | 2019-12-13 | 上海应用技术大学 | Preparation method of alkylation modified silica gel |
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