CN102912334A - Preparation method for high-stability nanometer silicon dioxide sol film coating solution - Google Patents
Preparation method for high-stability nanometer silicon dioxide sol film coating solution Download PDFInfo
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- CN102912334A CN102912334A CN2012103797257A CN201210379725A CN102912334A CN 102912334 A CN102912334 A CN 102912334A CN 2012103797257 A CN2012103797257 A CN 2012103797257A CN 201210379725 A CN201210379725 A CN 201210379725A CN 102912334 A CN102912334 A CN 102912334A
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Abstract
The invention discloses a preparation method for a high-stability nanometer silicon dioxide sol film coating solution. The preparation method comprises the steps as follows: firstly, preparing metal alkoxide, a solvent, water, a catalyst, a hydrolysis rate control agent and a film forming control agent according to the mass ratio of 5-30 to 47-85 to 1-5 to 0.5-2 to 3-10 to 5-12; secondly, uniformly dividing the solvent into two parts, mixing one part with the metal alkoxide to form a homogeneous phase solution A, and mixing another part with the water and the catalyst to form a homogeneous phase solution B; thirdly, dropwise adding the homogeneous phase solution B into the homogeneous phase solution A for hydrolytic condensation, stirring, sealing and curing to obtain alkaline silica sol with the pH value of 9-11; fourthly, adding the hydrolysis rate control agent, mixing, pouring into a triangular flask, condensing, reflowing and uniformly dropwise adding the film forming agent to obtain a sol sample with an additive; and lastly, adjusting the pH value of the sol sample to be 5-6 by using a pH value regulator. Under weak acid, the stability of nanometer silicon dioxide sol is greatly improved, the effective service life and the storage time of the sol are prolonged, and the problem of short gel time caused by poor stability of the conventional alkaline nanometer silicon dioxide sol is solved.
Description
Technical field
The present invention relates to photovoltaic glass and building glass coating technique field, be specifically related to a kind of preparation method of high-stability nano silicon dioxide gel coating liquid.
Background technology
In recent years, along with exploitation and the application of the various instruments such as large screen display, solar energy collector photovoltaic cell component, the research of glass antireflective effect more and more is subject to people's attention.Be exactly plated film on glass and make the anti-reflection a kind of simple effective method of glass.According to optical principle, plate the less film of one deck specific refractory power at glass substrate surface, the light transmission of substrate is improved.The surface protection glass of solar energy heating hydrophone for example, photovoltaic component packaging glass if improve by this method its light transmission, is conducive to improve photo-thermal transformation efficiency and electricity conversion.Present photovoltaic component encapsulating generally comprises glass substrate and anti-reflection film with glass, and anti-reflection film is coated in the glass substrate both sides or is subjected to a side of light, is used for improving the transmitance of packaged glass.Good uniformity, stoichiometric ratio are easily controlled because sol-gel method has, technique simply and aspect large-area applications, have advantage, industrial general employing sol-gel method prepares antireflecting silicon dioxide film colloidal sol.
But preparation has the most important condition that certain density high stable colloidal sol is preparation flawless, even structure film.Simultaneously the stability of colloidal sol be can the industrialization most critical precondition, stability is not enough, sometimes tends to produce silica dioxide gel in the preservation process.Gelation time is a very important parameter for sol-gel technology, and when the preparation film, the longer the better to wish gel time, can prolong like this effective storage life of colloidal sol.The common sol poor stability mainly is that the large or reunion degree difference of solid phase particles causes that particle size distribution is excessive to be caused.Its direct result is that film cracking, structure are inhomogeneous, even fully efflorescence.And the factor that affects gelation time is a lot, such as the PH of gelling system, TEOS concentration, system temperature etc.Wherein PH is the most remarkable on the collosol stability impact.
Summary of the invention
For solving above-mentioned problems of the prior art, order of the present invention is to provide a kind of preparation method of high-stability nano silicon dioxide gel coating liquid, has solved existing alkaline nano silicon dioxide gel and has caused the problem that gelation time is short because of poor stability.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of preparation method of high-stability nano silicon dioxide gel coating liquid comprises the steps:
Step 1: be equipped with starting material: metal alkoxide, solvent, water, catalyzer, hydrolysis rate control agent and filming control agent are equipped with metal alkoxide according to following mass percent: solvent: water: catalyzer: the hydrolysis rate control agent: the filming control agent is 5～30:47～85:1～5:0.5～2:3～10:5～12;
Step 2: solvent is divided into two parts, and portion mixes with metal alkoxide, stirs 0.5h～1h, makes it fully be mixed into homogeneous phase solution A, and another part and water and catalyst mix stir 0.5h～1h, make it fully be mixed into homogeneous phase solution B;
Step 3: homogeneous phase solution B is slowly dropped to the condensation that is hydrolyzed among the homogeneous phase solution A, stirred behind 6.0h～8.0h the sealing slaking 2～3 days, obtain pH value and be 9～11 alkaline silica sol;
Step 4: will be hydrolyzed control agent and slowly add in the alkaline silica sol that step 3 obtains, mix and blend 0.5h, then pour in the there-necked flask, 80 ℃～100 ℃ lower condensing reflux 6h～8h, with the ammonia volatile matter distillation, the test collosol PH value is 7～8, evenly drips subsequently membrane-forming agent, obtains the colloidal sol sample of additive;
Step 5: the colloidal sol sample that step 4 is obtained is adjusted to 5～6 with the pH value conditioning agent with pH value.
Described metal alkoxide is methyl silicate or tetraethoxy.
One or more mixing in described solvent methanol, ethanol, the Virahol, if multiple be for arbitrarily than mixing.
Described catalyzer is that mass concentration is 25%～38% ammoniacal liquor.
Described hydrolysis rate control agent is methyl ethyl diketone.
Described filming control agent is PVAC polyvinylalcohol, dimethyl formamide DMF or polyoxyethylene glycol.
Described pH value conditioning agent formic acid, acetic acid, hydrochloric acid or nitric acid.
The invention has the beneficial effects as follows: the nano silicon dioxide sol behind the condensing reflux is transferred to acid at 5 ~ 6 o'clock with PH, and the stability of colloidal sol improves greatly, and gelation time can extend to about 1 year.Collosol stability improves, the colloidal sol acceptable life prolongs, and the thickness of film and specific refractory power are easily controlled simultaneously shelf time prolongation in the film preparation process.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment one
The preparation method of a kind of high-stability nano silicon dioxide gel of the present embodiment coating liquid comprises the steps:
Step 1: take by weighing starting material: the quality that takes by weighing methyl silicate, methyl alcohol, water, concentration and be 25% ammoniacal liquor, methyl ethyl diketone and PVAC polyvinylalcohol is respectively 20.83g, 147g, 3.6g, 2g, 6g and 20.57g;
Step 2: methyl alcohol is divided into two parts, a mixes with methyl silicate, stirring 0.5h makes it fully be mixed into homogeneous phase solution A, and another part and water and mass concentration are that 25% ammoniacal liquor mixes, and stirring 0.5h makes it fully be mixed into homogeneous phase solution B;
Step 3: homogeneous phase solution B is slowly dropped to the condensation that is hydrolyzed among the homogeneous phase solution A, stirred behind the 6.0h sealing slaking 3 days, obtain pH value and be 9 alkaline silica sol;
Step 4: methyl ethyl diketone is slowly added in the alkaline silica sol that step 3 obtains, and then mix and blend 0.5h pours in the there-necked flask, 80 ℃ of lower condensing reflux 8h, with the ammonia volatile matter distillation, the test collosol PH value is 7, evenly drip subsequently PVAC polyvinylalcohol, obtain the colloidal sol sample of additive;
Step 5: the colloidal sol sample that step 4 is obtained is adjusted to 5 with formic acid with pH value.
Embodiment two
The preparation method of a kind of high-stability nano silicon dioxide gel of the present embodiment coating liquid comprises the steps:
Step 1: take by weighing starting material: the quality that takes by weighing methyl silicate, ethanol, water, concentration and be 30% ammoniacal liquor, methyl ethyl diketone and dimethyl formamide DMF is respectively 15.2g, 153.8g, 6g, 1g, 12g and 12g;
Step 2: ethanol is divided into two parts, a mixes with methyl silicate, stirring 0.8h makes it fully be mixed into homogeneous phase solution A, and another part and water and mass concentration are that 30% ammoniacal liquor mixes, and stirring 0.8h makes it fully be mixed into homogeneous phase solution B;
Step 3: homogeneous phase solution B is slowly dropped to the condensation that is hydrolyzed among the homogeneous phase solution A, stirred behind the 7.0h sealing slaking 2.5 days, obtain pH value and be 10 alkaline silica sol;
Step 4: methyl ethyl diketone is slowly added in the alkaline silica sol that step 3 obtains, and then mix and blend 0.5h pours in the there-necked flask, 90 ℃ of lower condensing reflux 7h, with the ammonia volatile matter distillation, the test collosol PH value is 7, evenly drip subsequently dimethyl formamide DMF, obtain the colloidal sol sample of additive;
Step 5: the colloidal sol sample that step 4 is obtained is adjusted to 6 with acetic acid with pH value.
Embodiment three
The preparation method of a kind of high-stability nano silicon dioxide gel of the present embodiment coating liquid comprises the steps:
Step 1: take by weighing starting material: the quality that takes by weighing tetraethoxy, Virahol, water, concentration and be 38% ammoniacal liquor, methyl ethyl diketone and polyoxyethylene glycol is respectively 40g, 103g, 9g, 4g, 20g and 24g;
Step 2: Virahol is divided into two parts, a mixes with tetraethoxy, stirring 1h makes it fully be mixed into homogeneous phase solution A, and another part and water and mass concentration are that 38% ammoniacal liquor mixes, and stirring 1h makes it fully be mixed into homogeneous phase solution B;
Step 3: homogeneous phase solution B is slowly dropped to the condensation that is hydrolyzed among the homogeneous phase solution A, stirred behind the 8.0h sealing slaking 2 days, obtain pH value and be 11 alkaline silica sol;
Step 4: methyl ethyl diketone is slowly added in the alkaline silica sol that step 3 obtains, and then mix and blend 0.5h pours in the there-necked flask, 100 ℃ of lower condensing reflux 6h, with the ammonia volatile matter distillation, the test collosol PH value is 8, evenly drip subsequently polyoxyethylene glycol, obtain the colloidal sol sample of additive;
Step 5: the colloidal sol sample that step 4 is obtained is adjusted to 6 with hydrochloric acid with pH value.
Claims (7)
1. the preparation method of a high-stability nano silicon dioxide gel coating liquid is characterized in that: comprise the steps:
Step 1: be equipped with starting material: metal alkoxide, solvent, water, catalyzer, hydrolysis rate control agent and filming control agent are equipped with metal alkoxide according to following mass percent: solvent: water: catalyzer: the hydrolysis rate control agent: the filming control agent is 5～30:47～85:1～5:0.5～2:3～10:5～12;
Step 2: solvent is divided into two parts, and portion mixes with metal alkoxide, stirs 0.5h～1h, makes it fully be mixed into homogeneous phase solution A, and another part and water and catalyst mix stir 0.5h～1h, make it fully be mixed into homogeneous phase solution B;
Step 3: homogeneous phase solution B is slowly dropped to the condensation that is hydrolyzed among the homogeneous phase solution A, stirred behind 6.0h～8.0h the sealing slaking 2～3 days, obtain pH value and be 9～11 alkaline silica sol;
Step 4: will be hydrolyzed control agent and slowly add in the alkaline silica sol that step 3 obtains, mix and blend 0.5h, then pour in the there-necked flask, 80 ℃～100 ℃ lower condensing reflux 6h～8h, with the ammonia volatile matter distillation, the test collosol PH value is 7～8, evenly drips subsequently membrane-forming agent, obtains the colloidal sol sample of additive;
Step 5: the colloidal sol sample that step 4 is obtained is adjusted to 5～6 with the pH value conditioning agent with pH value.
2. the preparation method of high-stability nano silicon dioxide gel coating liquid according to claim 1, it is characterized in that: described metal alkoxide is methyl silicate or tetraethoxy.
3. the preparation method of high-stability nano silicon dioxide gel coating liquid according to claim 1 is characterized in that: one or more mixing in described solvent methanol, ethanol, the Virahol, if multiple be for arbitrarily than mixing.
4. the preparation method of high-stability nano silicon dioxide gel coating liquid according to claim 1, it is characterized in that: described catalyzer is that concentration is 25%～38% ammoniacal liquor.
5. the preparation method of high-stability nano silicon dioxide gel coating liquid according to claim 1, it is characterized in that: described hydrolysis rate control agent is methyl ethyl diketone.
6. the preparation method of high-stability nano silicon dioxide gel coating liquid according to claim 1, it is characterized in that: described filming control agent is PVAC polyvinylalcohol, dimethyl formamide DMF or polyoxyethylene glycol.
7. the preparation method of high-stability nano silicon dioxide gel coating liquid according to claim 1 is characterized in that: described pH value conditioning agent formic acid, acetic acid, hydrochloric acid or nitric acid.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103725049A (en) * | 2013-12-03 | 2014-04-16 | 彩虹集团公司 | Preparation method for modified nano silicon dioxide coating liquid |
| CN104152032A (en) * | 2014-08-01 | 2014-11-19 | 苏州袭麟光电科技产业有限公司 | Scratch-resistant stiffed film and preparation method thereof |
| CN104278311A (en) * | 2014-09-30 | 2015-01-14 | 盐城工学院 | Preparation method of self-cleaning titanium dioxide nanotube array |
| CN105419631A (en) * | 2015-12-21 | 2016-03-23 | 中国航空工业集团公司北京航空材料研究院 | Composite sol coating material for surface of aluminum alloy, and preparation method and coating method thereof |
| CN106622047A (en) * | 2016-12-05 | 2017-05-10 | 浙江大学 | Metal element doped silicon dioxide alkaline nano sol and preparation method thereof |
| CN106811179A (en) * | 2017-01-03 | 2017-06-09 | 温州大学 | The preparation method of polyethylene glycol/silicon dioxide composite phase-change energy storage material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103725049A (en) * | 2013-12-03 | 2014-04-16 | 彩虹集团公司 | Preparation method for modified nano silicon dioxide coating liquid |
| CN104152032A (en) * | 2014-08-01 | 2014-11-19 | 苏州袭麟光电科技产业有限公司 | Scratch-resistant stiffed film and preparation method thereof |
| CN104278311A (en) * | 2014-09-30 | 2015-01-14 | 盐城工学院 | Preparation method of self-cleaning titanium dioxide nanotube array |
| CN105419631A (en) * | 2015-12-21 | 2016-03-23 | 中国航空工业集团公司北京航空材料研究院 | Composite sol coating material for surface of aluminum alloy, and preparation method and coating method thereof |
| CN106622047A (en) * | 2016-12-05 | 2017-05-10 | 浙江大学 | Metal element doped silicon dioxide alkaline nano sol and preparation method thereof |
| CN106811179A (en) * | 2017-01-03 | 2017-06-09 | 温州大学 | The preparation method of polyethylene glycol/silicon dioxide composite phase-change energy storage material |
| CN106811179B (en) * | 2017-01-03 | 2019-11-08 | 温州大学 | The preparation method of polyethylene glycol/silicon dioxide composite phase-change energy storage material |
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Application publication date: 20130206 |