CN105295446A - Method for preparing superhydrophobic powder - Google Patents
Method for preparing superhydrophobic powder Download PDFInfo
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- CN105295446A CN105295446A CN201410225058.6A CN201410225058A CN105295446A CN 105295446 A CN105295446 A CN 105295446A CN 201410225058 A CN201410225058 A CN 201410225058A CN 105295446 A CN105295446 A CN 105295446A
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Abstract
The invention relates to a method for preparing superhydrophobic powder. The method comprises the following steps: (1) preparing a SiO2-containing suspension; (2) preparing SiO2 nanoparticles; and (3) preparing the superhydrophobic powder: adding the SiO2 nanoparticles prepared in the step (2) and a silane coupling agent into an organic solvent, carrying out thorough mixing, then, carrying out stirring reaction for 15-20 hours at the temperature of 40-50 DEG C so as to obtain a suspension, then, standing the obtained suspension for 12-30 hours, removing supernatant liquid, and drying lower-layer precipitates, thereby obtaining the superhydrophobic powder, wherein the mass-to-volume ratio of the SiO2 nanoparticles to the silane coupling agent is 0.3-0.5g/10mL. According to the method disclosed by the invention, the preparation process is simple, the cost is low, and the prepared superhydrophobic powder is good in properties and has a broad application prospect in the fields of self-cleaning and the like.
Description
Technical field
The invention belongs to technical field of material, be specifically related to a kind of preparation method of super-hydrophobic powder.
Background technology
Occurring in nature, the surface of the plant such as lotus leaf, Rice Leaf presents hydrophobic performance because of the microtexture of its uniqueness and wax structure, and water droplet drops in leaf surfaces and forms spherical droplets immediately, rolls and takes away dust and bacterium.This super-hydrophobic phenomenon is derived from the low surface energy on its surface and unique roughness.Owing to having the surface property of many uniquenesses, as automatically cleaning, protection against corrosion, hydrophobicity etc., super-hydrophobic powder has using value in a lot of field, and such as add in paint, car wax or plastics, the surface that also directly can be coated in material makes it have self-cleaning function.The automatic cleaning coating of super-hydrophobic powder preparation can reduce the use of frequency of maintenance and water and sanitising agent.
In the world started to the research of super-hydrophobic material the 1950's, to late 1990s, along with the raising of the development especially study of surfaces technique means of Surface Science technology, imitate natural super hydrophobic material surface tissue and performance, prepare super-hydrophobic film and attract attention.The physical strength on artificial super hydrophobic material surface is not satisfactory at present, and long-term exposure in atmospheric environment time, be subject to the impact of various pollutent and dust, in addition the continuous action of the series of factors such as illumination, radiation, cause surface super hydrophobic performance to reduce and even lose; Also there is experiment condition harshness, complex steps, high in cost of production problem in the preparation method of the artificial super hydrophobic material of great majority, cannot industrial applications.Such as patent CN101646622B discloses a kind of method preparing hydrophobic aerogel, in acidic silicic acid sodium solution, add nonionogenic tenside, forms silica gel, in silica gel and mixed solvent, finally adds silicomethane agent react and prepare drainage powder.Its reaction process will under low pressure be carried out, and needs in fluid bed dispersion siccative dry.
Patent CN102925028A discloses a kind of preparation method of drainage powder coating, hydrophobic resin powder is carried out precomminution by high speed disintegrator, then melt extruded by twin screw extruder with nano-ceramic particle, finally high speed pulverization obtains drainage powder coating after sieving again.Its principle is, by physical method, the resin and nano-ceramic particle that possess hydrophobic performance are mixed to get drainage powder.Adopt nano-ceramic particle to be raw material in the method, cost is higher, and nano-ceramic particle will, through pre-treatment, need in preparation process repeatedly to pulverize, complex steps.
Summary of the invention
Technical problem to be solved by this invention is for above shortcomings in prior art, and provide a kind of preparation method of super-hydrophobic powder, cost is low, and technique is simple, is suitable for industrial production.
The present invention is for solving the problems of the technologies described above by the following technical solutions:
A preparation method for super-hydrophobic powder, it comprises the following steps:
(1) containing SiO
2the preparation of suspension liquid: positive silicon ester and small molecules monohydroxy-alcohol are added in deionized water, then drip ammonia soln adjust ph to 9.5 ~ 11, obtains containing SiO after reacting 4 ~ 7h under room temperature
2suspension liquid;
(2) SiO
2the preparation of nanoparticle: by step (1) gained containing SiO
2suspension liquid leaves standstill 12-30h, after its layering, remove supernatant liquid, and washs lower sediment thing with solvent, and then drying obtains SiO
2nanoparticle;
(3) preparation of super-hydrophobic powder: by the SiO of step (2) gained
2nanoparticle, silane coupling agent add in organic solvent, wherein SiO
2the mass volume ratio of nanoparticle and silane coupling agent is 0.3-0.5g/10mL, after abundant mixing at 40 ~ 50 DEG C stirring reaction 15 ~ 20h, obtain suspension liquid, then the suspension liquid of gained left standstill 12-30h, removing supernatant liquid, obtains super-hydrophobic powder by the drying of lower sediment thing.
By such scheme, step (1) described room temperature is 10-30 DEG C.
By such scheme, the described positive silicon ester of step (1) is methyl silicate, tetraethoxy or positive silicic acid propyl ester, is preferably tetraethoxy; Described small molecules monohydroxy-alcohol is methyl alcohol, ethanol, propyl alcohol or butanols, is preferably ethanol.
Preferably, step (1) drips ammonia soln adjust ph to 9.5.
By such scheme, the mol ratio of the described positive silicon ester of step (1) and small molecules monohydroxy-alcohol is 1:4.
By such scheme, step (2) described solvent is methyl alcohol, ethanol, propyl alcohol or ether, is preferably ethanol.
By such scheme, step (3) described silane coupling agent is trimethylchlorosilane; Step (3) described organic solvent is acetone or methyl iso-butyl ketone (MIBK).
By such scheme, step (2) and step (3) described drying are in an oven in 80 ~ 100 DEG C of dryings 24 hours, and preferred temperature is 80 DEG C.
By such scheme, step (3) the described stirring reaction time is preferably 16h.
The present invention also comprises the super-hydrophobic powder prepared according to aforesaid method, and described super-hydrophobic Powder Contact Angle is more than or equal to 170 °, for having nano-scale roughness, micron-scale particle diameter receive/super-hydrophobic the powder of micro-secondary structure.
Beneficial effect of the present invention is: 1, the present invention is reacted by positive silicon ester and small molecules monohydroxy-alcohol and prepares SiO
2nanoparticle, preparation method is simple, and do not use emulsifying agent and nano material, cost is low, and parameter is easy to control, and repeatability is high, is thus suitable for suitability for industrialized production; 2, the SiO for preparing of the present invention
2nano particle diameter is 20-100nm, carry out finishing further, by the effect of capillary force, solvation power etc., utilize the hydrophobic synergy of the hydrophobic and physics that is nano-micro structure of surface chemistry intrinsic to prepare and there is nano-scale roughness, micron-scale particle diameter receive/super-hydrophobic the powder of micro-secondary structure; 3, the contact angle of super-hydrophobic powder that prepared by the present invention reaches more than 170 °.
Accompanying drawing explanation
The water droplet shape appearance figure of the super-hydrophobic power applications of Fig. 1 prepared by the embodiment of the present invention 1 on slide glass;
The Flied emission scanning electron Electronic Speculum figure of the super-hydrophobic powder of Fig. 2 and Fig. 3 prepared by embodiment 1;
The super-hydrophobic powder of Fig. 4 prepared by embodiment 1 carries out the field emission scanning electron microscope figure after ultrasonic wave dispersion.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment of the present invention ammonia concn used is 25%.
Embodiment 1
(1) containing SiO
2the preparation of suspension liquid: 0.1mol tetraethoxy, 0.4mol dehydrated alcohol are mixed with 1.8mL deionized water, dripping ammoniacal liquor adjust ph is 9.5, reacts 6h and obtain white containing SiO under room temperature
2suspension liquid;
(2) SiO
2the preparation of nanoparticle: by gained containing SiO
2suspension liquid leaves standstill 24h, after its layering, remove supernatant liquid, and washs lower sediment thing with dehydrated alcohol, washs 3 times, and puts into 80 DEG C of dry 24h of baking oven and obtain SiO
2nanoparticle;
(3) preparation of super-hydrophobic powder: by 0.3gSiO
2nanoparticle, 10mL trimethylchlorosilane add in 20mL acetone, after abundant mixing at 50 DEG C stirring reaction 16h, obtain suspension liquid, then the suspension liquid of gained left standstill 24h, removing supernatant liquid, the dry 24h of baking oven lower sediment thing being put into 80 DEG C obtains super-hydrophobic powder.
The suspension liquid of contained for the present embodiment step (3) super-hydrophobic powder is spin-coated on slide glass, at 150 DEG C, dry 2h removes solvent and obtains hydrophobic membrane, recording its contact angle is 170 °, and the water droplet shape appearance figure of this super-hydrophobic power applications on slide glass as shown in Figure 1.Fig. 2-3 is scanning electron microscope (SEM) photographs of super-hydrophobic powder prepared by the present embodiment, show in figure, the super-hydrophobic powder of gained is for having nano-scale roughness (20-100nm), the particle of the receiving of micron-scale particle diameter/micro-secondary structure, it can thus be appreciated that, the SiO prepared by the present embodiment step (2)
2nano-particles size is 20-100nm.Fig. 4 is the field emission scanning electron microscope figure after the super-hydrophobic powder of the present embodiment gained carries out ultrasonic wave dispersion, as can be seen from the figure carries out the particle diameter of the rear super-hydrophobic powder of ultrasonic wave dispersion still at more than 500nm.Super-hydrophobic powder prepared by the present embodiment can be used as additive and uses, and also can directly apply to the surface of material.
Embodiment 2
(1) containing SiO
2the preparation of suspension liquid: 0.1mol methyl silicate, 0.4mol methyl alcohol are mixed with 1.8mL deionized water, dripping ammoniacal liquor adjust ph is 10, reacts 5h and obtain white containing SiO under room temperature
2suspension liquid;
(2) SiO
2the preparation of nanoparticle: by gained containing SiO
2suspension liquid leaves standstill 30h, after its layering, remove supernatant liquid, and washs lower sediment thing with methyl alcohol, washs 3 times, and puts into 100 DEG C of dry 24h of baking oven and obtain SiO
2nanoparticle;
(3) preparation of super-hydrophobic powder: by 0.3gSiO
2nanoparticle, 10mLTMCS (trimethylchlorosilane) add in 10mL acetone, after abundant mixing at 50 DEG C stirring reaction 20h, obtain suspension liquid, again the suspension liquid of gained is left standstill 12h, removing supernatant liquid, the dry 24h of baking oven lower sediment thing being put into 80 DEG C obtains super-hydrophobic powder.
Obtained super-hydrophobic powder morphology and hydrophobic performance similar to Example 1.
Embodiment 3
(1) containing SiO
2the preparation of suspension liquid: 0.1mol tetraethoxy, 0.4mol butanols are mixed with 1.8mL deionized water, dripping ammoniacal liquor adjust ph is 11, reacts 4h and obtain white containing SiO under room temperature
2suspension liquid;
(2) SiO
2the preparation of nanoparticle: by gained containing SiO
2suspension liquid leaves standstill 24h, after its layering, remove supernatant liquid, and washs lower sediment thing with propyl alcohol, washs 3 times, and puts into 90 DEG C of dry 24h of baking oven and obtain SiO
2nanoparticle;
(3) preparation of super-hydrophobic powder: by 0.6gSiO
2nanoparticle, 20mLTMCS (trimethylchlorosilane) add in 30mL methyl iso-butyl ketone (MIBK), after abundant mixing at 50 DEG C stirring reaction 15h, obtain suspension liquid, again the suspension liquid of gained is left standstill 30h, removing supernatant liquid, the dry 24h of baking oven lower sediment thing being put into 90 DEG C obtains super-hydrophobic powder.
Obtained super-hydrophobic powder morphology and hydrophobic performance similar to Example 1.
Embodiment 4
(1) containing SiO
2the preparation of suspension liquid: 0.1mol tetraethoxy, 0.4mol methyl alcohol are mixed with 3.6mL deionized water, dripping ammoniacal liquor adjust ph is 10, reacts 7h and obtain white containing SiO under room temperature
2suspension liquid;
(2) SiO
2the preparation of nanoparticle: by gained containing SiO
2suspension liquid leaves standstill 12h, after its layering, remove supernatant liquid, and washs lower sediment thing with ether, washs 4 times, and puts into 80 DEG C of dry 24h of baking oven and obtain SiO
2nanoparticle;
(3) preparation of super-hydrophobic powder: by 0.5gSiO
2nanoparticle, 10mLTMCS (trimethylchlorosilane) add in 20mL acetone, after abundant mixing at 40 DEG C stirring reaction 18h, obtain suspension liquid, again the suspension liquid of gained is left standstill 24h, removing supernatant liquid, the dry 24h of baking oven lower sediment thing being put into 90 DEG C obtains super-hydrophobic powder.
Obtained super-hydrophobic powder morphology and hydrophobic performance similar to Example 1.
Embodiment 5
(1) containing SiO
2the preparation of suspension liquid: positive for 0.1mol silicic acid propyl ester, 0.4mol dehydrated alcohol are mixed with 3.6mL deionized water, dripping ammoniacal liquor adjust ph is 10, reacts 6h and obtain white containing SiO under room temperature
2suspension liquid;
(2) SiO
2the preparation of nanoparticle: by gained containing SiO
2suspension liquid leaves standstill 24h, after its layering, remove supernatant liquid, and washs lower sediment thing with propyl alcohol, washs 4 times, and puts into 80 DEG C of dry 24h of baking oven and obtain SiO
2nanoparticle;
(3) preparation of super-hydrophobic powder: by 0.4gSiO
2nanoparticle, 10mLTMCS (trimethylchlorosilane) add in 10mL mibk, after abundant mixing at 40 DEG C stirring reaction 18h, obtain suspension liquid, again the suspension liquid of gained is left standstill 24h, removing supernatant liquid, the dry 24h of baking oven lower sediment thing being put into 100 DEG C obtains super-hydrophobic powder.
Obtained super-hydrophobic powder morphology and hydrophobic performance similar to Example 1.
Method provided by the invention prepares the little super-hydrophobic powder of particle diameter with easy steps as seen from the above embodiment, has scale operation prospect.
Be understandable that, the illustrative embodiments that above embodiment is only used to principle of the present invention is described and adopts, but the present invention is not limited thereto.For those skilled in the art, without departing from the spirit and substance in the present invention, can make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (6)
1. a preparation method for super-hydrophobic powder, is characterized in that comprising the following steps:
(1) containing SiO
2the preparation of suspension liquid: positive silicon ester and small molecules monohydroxy-alcohol are added in deionized water, then drip ammonia soln adjust ph to 9.5 ~ 11, obtains containing SiO after reacting 4 ~ 7h under room temperature
2suspension liquid;
(2) SiO
2the preparation of nanoparticle: by step (1) gained containing SiO
2suspension liquid leaves standstill 12-30h, after its layering, remove supernatant liquid, and washs lower sediment thing with solvent, and then drying obtains SiO
2nanoparticle;
(3) preparation of super-hydrophobic powder: by the SiO of step (2) gained
2nanoparticle, silane coupling agent add in organic solvent, wherein SiO
2the mass volume ratio of nanoparticle and silane coupling agent is 0.3-0.5g/10mL, after abundant mixing at 40 ~ 50 DEG C stirring reaction 15 ~ 20h, obtain suspension liquid, then the suspension liquid of gained left standstill 12-30h, removing supernatant liquid, obtains super-hydrophobic powder by the drying of lower sediment thing.
2. the preparation method of super-hydrophobic powder according to claim 1, is characterized in that: the described positive silicon ester of step (1) is methyl silicate, tetraethoxy or positive silicic acid propyl ester; Described small molecules monohydroxy-alcohol is methyl alcohol, ethanol, propyl alcohol or butanols.
3. the preparation method of super-hydrophobic powder according to claim 1 and 2, is characterized in that: the mol ratio of the described positive silicon ester of step (1) and small molecules monohydroxy-alcohol is 1:4.
4. the preparation method of super-hydrophobic powder according to claim 1, is characterized in that: step (2) described solvent is methyl alcohol, ethanol, propyl alcohol or ether.
5. the preparation method of super-hydrophobic powder according to claim 1, is characterized in that: step (3) described silane coupling agent is trimethylchlorosilane; Step (3) described organic solvent is acetone or methyl iso-butyl ketone (MIBK).
6. a super-hydrophobic powder, is characterized in that: according to the arbitrary described method preparation of claim 1-5, its contact angle is more than or equal to 170 °, for having nano-scale roughness, micron-scale particle diameter receive/super-hydrophobic the powder of micro-secondary structure.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106811957A (en) * | 2016-12-08 | 2017-06-09 | 苏州榕绿纳米科技有限公司 | A kind of preparation method of the super hydrophobic surface for for emulsion separate |
| CN108384284A (en) * | 2018-02-09 | 2018-08-10 | 航天特种材料及工艺技术研究所 | A kind of superhydrophobic inorganic material powder and preparation method thereof |
| CN110483818A (en) * | 2019-09-30 | 2019-11-22 | 三峡大学 | A kind of preparation method of the super-hydrophobic self-assembling function film of more particles |
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| CN103448116A (en) * | 2013-09-04 | 2013-12-18 | 东北林业大学 | Method for improving mechanical stability of super-hydrophobic wood |
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- 2014-05-26 CN CN201410225058.6A patent/CN105295446A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103448116A (en) * | 2013-09-04 | 2013-12-18 | 东北林业大学 | Method for improving mechanical stability of super-hydrophobic wood |
Non-Patent Citations (2)
| Title |
|---|
| A.VENKATESWARA RAO 等: ""Comparative studies on the surface chemical modification of silica aerogels based on various organosilane compounds of the type RnSiX4-n"", 《JOURNAL OF NON-CRYSTALLINE SOLIDS》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106811957A (en) * | 2016-12-08 | 2017-06-09 | 苏州榕绿纳米科技有限公司 | A kind of preparation method of the super hydrophobic surface for for emulsion separate |
| CN108384284A (en) * | 2018-02-09 | 2018-08-10 | 航天特种材料及工艺技术研究所 | A kind of superhydrophobic inorganic material powder and preparation method thereof |
| CN110483818A (en) * | 2019-09-30 | 2019-11-22 | 三峡大学 | A kind of preparation method of the super-hydrophobic self-assembling function film of more particles |
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Application publication date: 20160203 |