CN101704529B - Method for preparing amphiphilic nano silica powder and method for preparing Pickering emulsion using same - Google Patents

Method for preparing amphiphilic nano silica powder and method for preparing Pickering emulsion using same Download PDF

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CN101704529B
CN101704529B CN2009102186771A CN200910218677A CN101704529B CN 101704529 B CN101704529 B CN 101704529B CN 2009102186771 A CN2009102186771 A CN 2009102186771A CN 200910218677 A CN200910218677 A CN 200910218677A CN 101704529 B CN101704529 B CN 101704529B
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oil
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amphiphilic nano
silica powder
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CN101704529A (en
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范晓东
张卫红
田威
范伟伟
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Northwestern Polytechnical University
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Abstract

The invention discloses a method for preparing amphiphilic nano silica powder and is used for preparing nano silica powder with about 90 degrees of a tri-phase contact angle. The method uses ultrasonic preparation, thus having short preparation process; the invention adopts liquid phase modification, thus avoiding processing means such as grinding, calcining and the like which are easy to cause the powder to generate hard particle agglomeration; the invention can prepare better amphiphilic surface (about 90 degrees of tri-phase contact angle) nano silica powder. The invention also discloses a method for preparing Pickering emulsion by using the amphiphilic nano silica powder under the action of ultrasound or cutting, the nano silica powder stably exists in oil-water interface, thus preventing diffused oil (water) droplets to re-agglomerate into big droplets to split phase and stabilizing emulsion. The prepared emulsion can be stored at room temperature without occurrence of demulsification in three months.

Description

The preparation method of amphiphilic nano silica powder and the method that adopts this powder preparing Pickering emulsion
Technical field
The present invention relates to a kind of preparation method's of silicon-dioxide powdery, particularly amphiphilic nano silica powder preparation method.Also relate to the method that adopts this amphiphilic nano silica powder to prepare the Pickering emulsion.
Background technology
The Pickering emulsion often is called as solid (particle) stable form emulsion again, and the key that makes up such New Emulsion is the superfine powder that preparation has preferable amphipathic surface, nanometer SiO 2Powder is owing to nontoxic and have characteristics such as superior stability, reinforcement, thickening property and be fit to be used as stablizer and make up the Pickering emulsion.But general direct synthetic nano silicon contains great amount of hydroxy group and presents strongly hydrophilic owing to the surface, can not form stable Pickering emulsion.
Document 1 " K.Zhang, W.Wu, H.Meng et al.Pickering emulsion polymerization:Preparation ofpolystyrene/nano-SiO 2Composite microspheres with core-shell structure.Powder Technology 190 (2009) 393-400. " disclose a kind of with methyl allyl acyloxypropyl trimethoxysilane (KH570) modified Nano SiO 2Method, the contact angle of gained powder is 38.5 °, only can form the Pickering emulsion under the acidic conditions of pH=3, and stability is not good enough, storing 24h promptly has obvious demixing phenomenon to take place.
Document 2 " publication number is the Chinese invention patent of CN 1724352A " discloses a kind of preparation method of amphiphilic nano silicon dioxide, adopt amphipathic block polyether finishing to prepare amphiphilic nano silica, but need in the whole process of preparation through anion and cation exchange resin handle, repeatedly regulate the pH value, leave standstill, steps such as reaction and ultrafiltration and concentration, consuming time longer, operation easier is also bigger.
Summary of the invention
In order to overcome the nanometer SiO of prior art for preparing 2The deficiency that surface contact angle is little the invention provides a kind of amphiphilic nano SiO 2The preparation method of powder, adopt the liquid phase modification, can avoid grinding, calcining etc. easily makes powder produce the processing means of hard aggregation, by the pH value of control dispersion liquid and the add-on of silane coupling agent, can prepare nano silica powder with about 90 ° of preferable amphipathic surface contact angles.
In order to overcome prior art nanometer SiO 2The deficiency that the Pickering emulsion storage time of preparation is short, the present invention also provides and adopts aforementioned amphiphilic nano SiO 2The method of powder preparing Pickering emulsion, amphiphilic nano SiO 2Powder ultra-sonic dispersion in advance adds oil-based solvent (or water) then according to a certain volume in water (or oil phase), large power supersonic or high speed shear emulsification can make stable O/W (or W/O) type Pickering emulsion.
The technical solution adopted for the present invention to solve the technical problems: a kind of amphiphilic nano SiO 2The preparation method of powder is characterized in comprising the steps:
(a) tetraethoxy, ammoniacal liquor, methyl alcohol were mixed in 1: 2: 30 by volume, ultrasonic reaction 2～5h, ultrasound condition: frequency 30～60KHz, power 200～300W, temperature is controlled at 15 ℃～25 ℃ in the reaction process, obtains the nano silicon dispersion liquid;
(b) get the nano silicon dispersion liquid that step (a) prepares, under pH meter monitoring and magnetic agitation, dropwise add glacial acetic acid, regulating the pH value is 7～7.5, the chain alkyl Trimethoxy silane coupling agent that adds dispersion liquid volume fraction 0.09%～0.15% then, at 70 ℃～90 ℃ following back flow reaction 3～4h, 20000～25000r/min is centrifugal, back dehydrated alcohol ultrasonic cleaning, and then it is centrifugal, ultrasonic cleaning, this step repeats 3～5 times, with gained spawn vacuum-drying 8～10h under 20～40 ℃ of conditions, take out slightly grind amphiphilic nano SiO 2Powder.
The above-mentioned amphiphilic nano SiO of a kind of employing 2Powder is made the method for Pickering emulsion, it is characterized in that may further comprise the steps:
Get amphiphilic nano SiO 2Powder, by powder: the mass/volume ratio of water=1: 100～1: 150 adds in the entry, ultra-sonic dispersion 20～30min, ultrasound condition: frequency 30～60KHz, power 200～300W, again to wherein by oil: the volume ratio of water=1: 10～1: 15 adds oil-based solvent, is that 75～85% ultrasonic cell pulverization machine is pulverized through amplitude, be high speed shear emulsification instrument processing 2～3min of 18000～23000r/min perhaps, promptly get oil-in-water-type Pickering emulsion through rotating speed;
Perhaps get amphiphilic nano SiO 2Powder, press powder: the mass/volume of oil=1: 100～1: 50 is than adding in the oil-based solvent, ultra-sonic dispersion 20～30min, ultrasound condition: frequency 30～60KHz, power 200～300W, again to wherein by water: the volume ratio of oil=1: 7.5～1: 10 adds entry, is that 75～85% ultrasonic cell pulverization machine is pulverized through amplitude, be high speed shear emulsification instrument processing 2～3min of 18000～23000r/min perhaps, promptly get water-in-oil-type Pickering emulsion through rotating speed.
Described oil-based solvent is any of normal heptane, benzene, toluene, propyl carbinol, isopropylcarbinol or ethyl acetate.
The invention has the beneficial effects as follows: adopt ultrasonic preparation nano silica powder, preparation process is short; Adopt the liquid phase modification, avoided grinding, calcining etc. easily to make powder produce the processing means of hard aggregation, only just prepared nano silicon with preferable amphipathic surface (about 90 ° of three-phase contact angles) by the pH value of control dispersion liquid and the add-on of silane coupling agent, gained powder hard aggregation-free reaches nano level easily and disperses under ultrasonication.
Owing to adopt the amphiphilic nano silica powder of contact angle about 90 °, preparation O/W or w/o type Pickering emulsion under ultrasonic or shearing action, nano silica powder is stable is present in water-oil interface, stop dispersive oil (water) droplet to condense once more and be big drop phase-splitting, make emulsion keep stable, deposit under the made emulsion room temperature and do not occur obvious demulsifying phenomenon in 3 months.
Below in conjunction with drawings and Examples the present invention is elaborated.
Description of drawings
Fig. 1 is the prepared nanometer SiO of embodiment 1 2The nanometer SiO of powder and background technology preparation 2Granularity and size-grade distribution laser particle analyzer detect figure.
Fig. 2 is the prepared nanometer SiO of embodiment 2 2The nanometer SiO of powder and background technology preparation 2The laser particle size detected result.
Fig. 3 is the prepared nanometer SiO of embodiment 2 2The nanometer SiO of powder and background technology preparation 2Infrared contrast collection of illustrative plates.
Fig. 4 is the prepared nanometer SiO of embodiment 3 2The nanometer SiO of powder and background technology preparation 2The laser particle size detected result.
Fig. 5 is the prepared nanometer SiO of embodiment 4 2The nanometer SiO of powder and background technology preparation 2The laser particle size detected result.
Embodiment
Embodiment 1: get 20mL tetraethoxy and 200mL methyl alcohol, at frequency 40KHz, shake 5min in the power 250W ultrasonic cleaner; Getting 40mL concentration and be 25% ammoniacal liquor joins in the 400mL methyl alcohol, just be poured into after stirring ultrasonic concussion the methanol solution of tetraethoxy in, at the ultrasonic reaction 3h that continues down, whole process adopts the recirculated water cooling, keep water temperature at 15 ℃, finally can obtain nattier blue nanometer SiO 2Dispersion liquid.Detect through laser particle analyzer, Z-Average (d.nm): 42.8nm, granularity heterogeneity index (PDI) is 0.149, detected result is seen Fig. 1.This dispersion liquid stable in properties deposits at room temperature that particle diameter does not change substantially more than 3 months.
Get above-mentioned nanometer SiO 2Dispersion liquid 100mL, under pH meter monitoring and magnetic agitation, drip glacial acetic acid, regulating dispersion liquid pH value is 7.0, add 0.12mL chain alkyl Trimethoxy silane (WD-10) behind the ultra-sonic dispersion 10min, ultra-sonic dispersion 5min again, then with dispersion liquid at 80 ℃ of following back flow reaction 4h, through 20000r/min high speed centrifugation 15min, remove supernatant liquor and obtain pale blue transparent gel-form modification SiO 2, adding the ultrasonic rinsing 10min of 10mL dehydrated alcohol, recentrifuge and ultrasonic rinsing 3～5 times repeatedly, place vacuum drying oven dry 10h under 20 ℃ to get amphiphilic nano SiO final centrifugal product 2Take out slightly grind amphiphilic nano SiO 2Powder.Granularity and size-grade distribution result are after testing: Z-Average (d.nm): 86.4nm; PDI:0.197 sees Fig. 1.
Getting above-mentioned pressed by powder diameter is
Figure G2009102186771D00031
The thin slice of the about 2mm of thickness, ironed of institute is placed in the transparent vessel, add the whiteruss submergence, about the high 1cm of submergence liquid level, drip water on the subsurface thin slice of paraffin with dropper, treat that drop takes pictures with digital camera immediately after stable on the thin slice, test its three-phase contact angle subsequently, the result is 85 °-90 °.
Get 0.3g amphiphilic nano SiO 2Powder adds in the 30mL water, and (30KHz, 300W) 20min to wherein adding 2mL toluene, pulverize 2min through ultrasonic cell pulverization machine (500W, 85% amplitude) to ultra-sonic dispersion again, can form stable oil-in-water (O/W) type Pickering emulsion.This emulsion property is stable, and demulsifying phenomenon did not appear in 3 months in airtight placement under the room temperature.
Embodiment 2: get 10mL tetraethoxy and 100mL methyl alcohol, at frequency 30KHz, shake 6min in the power 300W ultrasonic cleaner; Getting 20mL concentration and be 26% ammoniacal liquor joins in the 200mL methyl alcohol, just be poured into after stirring ultrasonic concussion the methanol solution of tetraethoxy in, at the ultrasonic reaction 2h that continues down, whole process adopts the recirculated water cooling, keep water temperature at 18 ℃, finally can obtain nattier blue nanometer SiO 2Dispersion liquid.Detect through laser particle analyzer, Z-Average (d.nm): 44.1nm, granularity heterogeneity index (PDI) is 0.157, sees Fig. 2.
Get above-mentioned nanometer SiO 2Dispersion liquid 100mL, under pH meter monitoring and magnetic agitation, drip glacial acetic acid, regulating dispersion liquid pH value is 7.3, add 0.15mL chain alkyl Trimethoxy silane (WD-10) behind the ultra-sonic dispersion 10min, ultra-sonic dispersion 5min again, then with dispersion liquid at 70 ℃ of following back flow reaction 3h, through 25000r/min high speed centrifugation 16min, remove supernatant liquor and obtain pale blue transparent gel-form modification SiO 2, adding the ultrasonic rinsing 10min of 10mL dehydrated alcohol, recentrifuge and ultrasonic rinsing 3～5 times repeatedly, place vacuum drying oven dry 9h under 25 ℃ to get amphiphilic nano SiO final centrifugal product 2Take out slightly grind amphiphilic nano SiO 2Powder.Granularity and size-grade distribution result are after testing: Z-Average (d.nm): 84.6nm; PDI:0.160 sees Fig. 2.SiO before modified powder and the modification 2Carry out infrared spectra respectively and detect, as shown in Figure 3,3400cm -1The place is the hydroxyl peak of planar water and powder surface, 1100cm -1, 800cm -1And 470cm -1Adhere to Si-O-Si skeletal vibration, asymmetric and symmetrical stretching vibration peak separately, be SiO 2Characteristic peak; Different is that after the modification of chain alkyl Trimethoxy silane, modified powder is at 2927cm -1And 2855cm -1Absorption peak has to a certain degree appearred in the place, these two peak correspondences be methylene radical (CH 2) C-H unsymmetrically and symmetrical stretching vibration peak, this shows has alkyl to be attached to powder surface with the form of chemical bond.
Getting above-mentioned pressed by powder diameter is
Figure G2009102186771D00041
The thin slice of the about 2mm of thickness, ironed of institute is placed in the transparent vessel, add the whiteruss submergence, about the high 1cm of submergence liquid level, drip water on the subsurface thin slice of paraffin with dropper, treat that drop takes pictures with digital camera immediately after stable on the thin slice, test its three-phase contact angle subsequently, the result is 90 °-95 °.
Get 0.3g amphiphilic nano SiO 2Powder adds in the 30mL ethyl acetate, and (40KHz, 260W) 24min to wherein adding the 2mL pure water, handle 2min through high speed shear emulsification instrument (23000r/min) to ultra-sonic dispersion again, can form stable water-in-oil (W/O) type Pickering emulsion.
Embodiment 3: get 30mL tetraethoxy and 300mL methyl alcohol, at frequency 60KHz, shake 8min in the power 200W ultrasonic cleaner; Getting 60mL concentration and be 27% ammoniacal liquor joins in the 600mL methyl alcohol, just be poured into after stirring ultrasonic concussion the methanol solution of tetraethoxy in, at the ultrasonic reaction 5h that continues down, whole process adopts the recirculated water cooling, keep water temperature at 21 ℃, finally can obtain nattier blue nanometer SiO 2Dispersion liquid.Detect through laser particle analyzer, Z-Average (d.nm): 43.2nm, granularity heterogeneity index (PDI) is 0.173, sees Fig. 4.
Get above-mentioned nanometer SiO 2Dispersion liquid 100mL, under pH meter monitoring and magnetic agitation, drip glacial acetic acid, regulating dispersion liquid pH value is 7.5, add 0.09mL chain alkyl Trimethoxy silane (WD-10) behind the ultra-sonic dispersion 10min, ultra-sonic dispersion 5min again, then with dispersion liquid at 80 ℃ of following back flow reaction 3.5h, through 21000r/min high speed centrifugation 18min, remove supernatant liquor and obtain pale blue transparent gel-form modification SiO 2, adding the ultrasonic rinsing 10min of 10mL dehydrated alcohol, recentrifuge and ultrasonic rinsing 3～5 times repeatedly, place vacuum drying oven dry 8h under 30 ℃ to get amphiphilic nano SiO final centrifugal product 2Take out slightly grind amphiphilic nano SiO 2Powder.Granularity and size-grade distribution result are after testing: Z-Average (d.nm): 86.6nm; PDI:0.205 sees Fig. 4.
Getting above-mentioned pressed by powder diameter is
Figure G2009102186771D00042
The thin slice of the about 2mm of thickness, ironed of institute is placed in the transparent vessel, add the whiteruss submergence, about the high 1cm of submergence liquid level, drip water on the subsurface thin slice of paraffin with dropper, treat that drop takes pictures with digital camera immediately after stable on the thin slice, test its three-phase contact angle subsequently, the result is 85 °-88 °.
Get 0.1g amphiphilic nano SiO 2Powder adds in the 15mL water, and (50KHz, 220W) 27min to wherein adding the 1.5mL normal heptane, pulverize 3min through ultrasonic cell pulverization machine (500W, 75% amplitude) to ultra-sonic dispersion again, can form stable oil-in-water (O/W) type Pickering emulsion.
Embodiment 4: get 20mL tetraethoxy and 200mL methyl alcohol, at frequency 40KHz, shake 10min in the power 250W ultrasonic cleaner; Getting 40mL concentration and be 28% ammoniacal liquor joins in the 400mL methyl alcohol, just be poured into after stirring ultrasonic concussion the methanol solution of tetraethoxy in, at the ultrasonic reaction 4h that continues down, whole process adopts the recirculated water cooling, keep water temperature at 25 ℃, finally can obtain nattier blue nanometer SiO 2Dispersion liquid.Detect through laser particle analyzer, Z-Average (d.nm): 36.2nm, granularity heterogeneity index (PDI) is 0.162, sees Fig. 5.
Get above-mentioned nanometer SiO 2Dispersion liquid 100mL, under pH meter monitoring and magnetic agitation, drip glacial acetic acid, regulating dispersion liquid pH value is 7.4, add 0.11mL chain alkyl Trimethoxy silane (WD-10) behind the ultra-sonic dispersion 10min, ultra-sonic dispersion 5min again, then with dispersion liquid at 75 ℃ of following back flow reaction 4h, through 23000r/min high speed centrifugation 15min, remove supernatant liquor and obtain pale blue transparent gel-form modification SiO 2, adding the ultrasonic rinsing 10min of 10mL dehydrated alcohol, recentrifuge and ultrasonic rinsing 3～5 times repeatedly, place vacuum drying oven dry 8h under 40 ℃ to get amphiphilic nano SiO final centrifugal product 2Take out slightly grind amphiphilic nano SiO 2Powder.Granularity and size-grade distribution result are after testing: Z-Average (d.nm): 80.4nm; PDI:0.137 sees Fig. 5.
Getting above-mentioned pressed by powder diameter is
Figure G2009102186771D00051
The thin slice of the about 2mm of thickness, ironed of institute is placed in the transparent vessel, add the whiteruss submergence, about the high 1cm of submergence liquid level, drip water on the subsurface thin slice of paraffin with dropper, treat that drop takes pictures with digital camera immediately after stable on the thin slice, test its three-phase contact angle subsequently, the result is 90 °-95 °.
Get 0.3g amphiphilic nano SiO 2Powder adds in the 15mL isopropylcarbinol, and (60KHz, 200W) 30min to wherein adding the 2mL pure water, handle 3min through high speed shear emulsification instrument 23000r/min to ultra-sonic dispersion again, can form stable water-in-oil (W/O) type Pickering emulsion.
In addition, also test with oil-based solvents such as benzene, propyl carbinols respectively, all obtained good effect.

Claims (2)

1. amphiphilic nano SiO 2The preparation method of powder is characterized in that may further comprise the steps:
(a) tetraethoxy, ammoniacal liquor, methyl alcohol were mixed in 1: 2: 30 by volume, ultrasonic reaction 2～5h, ultrasound condition: frequency 30～60KHz, power 200～300W, temperature is controlled at 15 ℃～25 ℃ in the reaction process, obtains the nano silicon dispersion liquid;
(b) get the nano silicon dispersion liquid that step (a) prepares, under pH meter monitoring and magnetic agitation, dropwise add glacial acetic acid, regulating the pH value is 7～7.5, the chain alkyl Trimethoxy silane coupling agent that adds dispersion liquid volume fraction 0.09%～0.15% then, at 70 ℃～90 ℃ following back flow reaction 3～4h, 20000～25000r/min is centrifugal, back dehydrated alcohol ultrasonic cleaning, and then it is centrifugal, ultrasonic cleaning, this step repeats 3～5 times, with gained spawn vacuum-drying 8～10h under 20～40 ℃ of conditions, take out slightly grind amphiphilic nano SiO 2Powder.
2. one kind is adopted the described amphiphilic nano SiO of claim 1 2The prepared amphiphilic nano SiO of the preparation method of powder 2Powder is made the method for Pickering emulsion, it is characterized in that may further comprise the steps:
Get amphiphilic nano SiO 2Powder, by powder: the mass/volume ratio of water=1: 100～1: 150 adds in the entry, ultra-sonic dispersion 20～30min, ultrasound condition: frequency 30～60KHz, power 200～300W, again to wherein by oil: the volume ratio of water=1: 10～1: 15 adds oil-based solvent, is that 75～85% ultrasonic cell pulverization machine is pulverized through amplitude, be high speed shear emulsification instrument processing 2～3min of 18000～23000r/min perhaps, promptly get oil-in-water-type Pickering emulsion through rotating speed;
Perhaps get amphiphilic nano SiO 2Powder, press powder: the mass/volume of oil=1: 100～1: 50 is than adding in the oil-based solvent, ultra-sonic dispersion 20～30min, ultrasound condition: frequency 30～60KHz, power 200～300W, again to wherein by water: the volume ratio of oil=1: 7.5～1: 10 adds entry, is that 75～85% ultrasonic cell pulverization machine is pulverized through amplitude, be high speed shear emulsification instrument processing 2～3min of 18000～23000r/min perhaps, promptly get water-in-oil-type Pickering emulsion through rotating speed;
Described oil-based solvent is any of normal heptane, benzene, toluene, propyl carbinol, isopropylcarbinol or ethyl acetate.
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