CN105347693A - Long-acting glass hydrophobic agent and preparation and application method thereof - Google Patents
Long-acting glass hydrophobic agent and preparation and application method thereof Download PDFInfo
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- CN105347693A CN105347693A CN201410418605.2A CN201410418605A CN105347693A CN 105347693 A CN105347693 A CN 105347693A CN 201410418605 A CN201410418605 A CN 201410418605A CN 105347693 A CN105347693 A CN 105347693A
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Abstract
The invention discloses a long-acting glass hydrophobic agent and its preparation and application method, and relates to the technical field of glass hydrophobic treatment. According to the invention, high-molecular-weight polysiloxane with a certain branched structure, which is used as a main raw material, is mixed with an acid catalyst and a corresponding solvent, so as to prepare the hydrophobic agent. When the hydrophobic agent is used to process glass surface, the material's molecular chain can further undergo polymerization for growth or crosslinking under the action of a catalyst and main chain and side chain undergo crossed entanglement; meanwhile, through chemical bond combination on the glass surface and with the cooperation of polymer viscosity and winding mechanical force, a tightly-combined protective film is formed. The protective film can have rain-proof, oil-resistant, freezing-rain-proofing, frost-proof and self-cleaning effects, is solvent-resistant and wash-resistant, and shows excellent durability. Meanwhile, the product doesn't affect glass quality and will not have any adverse effect on sight (such as reflection of light, blurring, etc.).
Description
Technical field
The present invention relates to glass hydrophobic treatment technical field, refer to a kind of long-acting glass hydrophobizing agent and preparation and application thereof especially.
Background technology
Surface of ordinary glass is water-wetted surface, the light transmission of glass can be made to be deteriorated, and windshield, side windshield glass and front and back visor is fuzzy, is the major reason causing traffic accident when water droplet is expanded on glass.When rain or high humidity vehicle glass surface just can form the drips sight line of attachment.Existing main solution is for using wiper and the timely wiping of rag, and this method is also inconvenient, can not solve root problem.
In the market, can scribble hydrophobic coating to solve the problem of rainy day traveling at its glass surface when most of automobile dispatches from the factory, but its complete processing is complicated, hydrophobic effect has some limitations.Meanwhile, market also exists routine vehicle maintenance glass hydrophobizing agent, but it is generally fugitive hydrophobizing agent, and is mainly fluorine-containing type siloxane product, have that raw material sources are limited, high expensive, the problem such as not environmentally.
Domestic scientific research personnel does a lot in the research and development of floride-free hydrophobizing agent, as patent CN1778749A discloses a kind of glass hydrophobic film coating liuqid based on long chain alkyl silane coupling agent and alkyl silicate, this utilizes small molecules silane monomer to construct hydrophobic coating in glass surface reaction.But small molecules coating is low at low temperature, the coating mechanical strength that generates in the short period of time, easily weares and teares, is difficult to use in daily quick maintenance, can not ensures enough persistence.Patent CN101148325A adds inorganic nanoparticles on the basis of the above, but the feature that nano particle is easily reunited due to self can produce inevitable scattering process to visible ray, cannot realize real coating transparent.
Abroad, Trevisan etc. have invented a kind of method (U.S. Patent number No.3,958,073) that effectively can prevent glass surface hydrolysis and chemical reagent enrichment, have good waterproof efficacy, its main component is made up of compound such as borosilicate acid esters, titanium, zirconium, tin.After glass surface has smeared this product, toast at 200 ~ 400 DEG C, just can obtain the splendid glass of hydrophobic effect, this treatment process complex process, equipment requirements are high, cannot use in actual daily maintenance.
Therefore, finding one can use at ambient temperature, and the glass hydrophobizing agent for a long time with effects such as waterproof, dedusting are self-cleaning is the focus of research.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of novel long-acting glass hydrophobizing agent based on macromolecule polysiloxane and preparation and application thereof.High polysiloxane in hydrophobizing agent is Main Function composition, rely on the force of cohesion of molecule self, entanglement mechanical force, oilness and hydrophobicity, and reach long-acting, hydrophobic with the Chemical bonding of substrate of glass, dedusting, the effect such as self-cleaning, and, this hydrophobizing agent can at room temperature directly use, easy and simple to handle.
For solving the problems of the technologies described above, the invention provides technical scheme as follows:
On the one hand, a kind of long-acting glass hydrophobizing agent is provided, is made up of by weight percentage following compositions:
Macromolecule polysiloxane is 0.5 ~ 20wt%;
An acidic catalyst is 0.5 ~ 3wt%;
Solvent 77 ~ 98wt%.
Further, described macromolecule polysiloxane and an acidic catalyst weight ratio are 3:1 ~ 25:1, account for 2% ~ 15% of gross weight altogether.
Further, described macromolecule polysiloxane is the polysiloxane that molecular chain-end has active function groups end-blocking, described active function groups be selected from alkoxyl group, amino, hydroxyl, sulfydryl, chlorine substituent, bromine substituent, epoxy group(ing) one or more.
Further preferred, described macromolecule polysiloxane be molecular chain-end there is active function groups end-blocking there are one or more of the long-chain siloxane polymer of certain branched structure, its structural formula general formula can be expressed as:
Wherein x value is 6 ~ 40, y value be 5 ~ 20, z value be 5 ~ 30, n value is 0 ~ 8; R
1, R
2, R
3for active function groups, be selected from the one in alkoxyl group, amino, hydroxyl, sulfydryl, chlorine atom, bromine atoms, epoxy group(ing), can identical also can be different.
Further, described an acidic catalyst is one or more in acetic acid, hydrochloric acid, nitric acid, sulfuric acid.
Further, solvent is one or more in water, acetonitrile, acetone, methyl alcohol, ethanol, Virahol, propyl carbinol, isopropylcarbinol.
On the other hand, a kind of preparation method of above-mentioned long-acting glass hydrophobizing agent is provided, above-mentioned polysiloxane and an acidic catalyst is added hybrid reaction in solvent and obtains target product.Preparation method's temperature of reaction of the present invention is-10 ~ 80 DEG C, and the reaction times is 1-24h.
Further, mixing step specifically comprises: step 1: an acidic catalyst and solvent are obtained acidic medium; Step 2: stir in described acidic medium and slowly add described polysiloxane hybrid reaction, obtained described long-acting glass hydrophobizing agent.
Again on the one hand, a kind of using method of above-mentioned long-acting glass hydrophobizing agent is provided, comprises:
Step 1: by glass surface scrub;
Step 2: hydrophobizing agent is evenly coated in glass surface, at room temperature leaves standstill and waits until to dry and occur white film;
Step 3: with clean cotton cleaning glass window surface, be polished to bright and clean seamless.
Further, step 1 is all at room temperature carried out to step 3.
Long-acting glass hydrophobizing agent of the present invention, can form layer of transparent, opaque plated film at glass surface, and be connected with molecule covalent key form with glass surface, form firmly protective membrane, can not lose efficacy because of external force such as rain brush.The sleet that this hydrophobizing agent drops under can effectively impelling on vehicle glass forms water droplet and tumbles with the wind rapidly, ensures automobile rainy day driving visibility meter, guarantee driving safety.It can effectively avoid frost, greasy dirt, dust etc. in the attachment of glass surface, makes the secondary of glass clean very convenient.Be applicable to outside windshield, side window and rear window outer surface, the glass surface treatment such as rear vision mirror surface, fog lamp, headlight surface, Domestic window glass, bathroom glass, mirror, high-rise glass.
The present invention is with macromolecule polysiloxane for Main Function composition, and the feature of the high cohesion utilizing long chain macromolecule self intrinsic, high viscosity, easy entanglement, provides stronger sticking power and more excellent scratch-resistant performance.In addition, the active function groups at polysiloxane molecule chain two ends can issue raw intermolecular chainpropagation and chain is cross-linked in the effect of an acidic catalyst, simultaneously when it is coated on glass surface, also can react with glass surface and be connected with molecule covalent key form, further enhance polysiloxane network at suprabasil adhesion effect.Consume because active function groups reacts, hydrophobic alkane segment, the silica segment of low surface energy can cover glass surface completely with the form of staggered-mesh, provide effect of excellent waterproof, anti-electrostatic, anti-dirt adhesion.
Comprehensively above-mentioned, beneficial effect of the present invention shows as:
1) long-acting glass hydrophobizing agent, has strong-hydrophobicity and low surface energy, is covered in that glass surface avoids the water of active group, frost, greasy dirt and mud dirt etc. directly contact with glass surface thus above being attached to.
2) long-acting glass hydrophobizing agent of the present invention, is acted synergistically mutually by self chainpropagation, entanglement and being connected with glass surface molecule covalent, and form the protective membrane of mortise, can not lose efficacy because of external force such as rain brush, window brushes, hydrophobic effect is lasting.
3) long-acting glass hydrophobizing agent of the present invention does not affect glass quality, also can not produce any impact (as reflective, smudgy etc.) to sight line.
4) long-acting glass hydrophobizing agent of the present invention does not adopt fluorine-containing silicane raw material, produce and use cost low, can extensively promotion and application.
5) preparation method of the long-acting glass hydrophobizing agent of the present invention and use, easy and simple to handle, is easy to realize, and is widely used.
Accompanying drawing explanation
Fig. 1 a-Fig. 1 b is respectively the static contact angle contrast of the glass surface before and after surface of ordinary glass hydrophobic treatment.
Fig. 2 a-Fig. 2 b is respectively the transmittance change curve of simple glass before and after process of the present invention under Different lightwave is long.
Fig. 3 is the static contact angle Data Comparison that simple glass carries out circulation rub(bing)test respectively after the present invention and the process of available glass hydrophobizing agent.Wherein, solid dot curve is the data and curves through process of the present invention, and hollow dots is the data and curves of contrast hydrophobizing agent.
Fig. 4 is that simple glass is placed on the static contact angle data and curves of different time test in outdoor environment through process of the present invention.
Embodiment
For making the technical problem to be solved in the present invention, technical scheme and advantage clearly, below specific embodiment is described in detail.But the present invention is limited to absolutely not these examples.The following stated is only the good embodiment of the present invention, only in order to explain the present invention, therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Embodiment one:
Long-acting glass hydrophobizing agent of the present invention is prepared according to following formula and ratio:
Preparation method:
A) in 79g dehydrated alcohol and 15g Virahol mixed solution, add 1g hydrochloric acid, stir 30min.
B) in a) step solution, slowly add 5g polysiloxane while stirring, room temperature continues to stir 3h, just can obtain required long-acting glass hydrophobizing agent.
Embodiment two:
Long-acting glass hydrophobizing agent of the present invention is prepared according to following formula and ratio:
Preparation method:
A) slowly add 1g sulfuric acid to 85g dehydrated alcohol and 4g Virahol mixed solution, stir 30min.
B) in a) step solution, slowly add 10g polysiloxane while stirring, room temperature continues to stir 6h, just can obtain required long-acting glass hydrophobizing agent.
Embodiment three:
Long-acting glass hydrophobizing agent of the present invention is prepared according to following formula and ratio:
Preparation method:
A) in the mixed solution of 95g dehydrated alcohol and 1g water, slowly add 1g sulfuric acid, stir 30min.
B) in a) step solution, slowly add 3g polysiloxane while stirring, continue to stir 4h at 40 DEG C, just can obtain required long-acting glass hydrophobizing agent.
Embodiment four:
Long-acting glass hydrophobizing agent of the present invention is prepared according to following formula and ratio:
Preparation method:
A) in the mixed solution of 85g dehydrated alcohol and 2g acetone, slowly add 0.5g nitric acid, stir 30min.
B) in a) step solution, slowly add 12.5g polysiloxane while stirring, continue to stir 6h at 30 DEG C, just can obtain required long-acting glass hydrophobizing agent.
Embodiment five:
Long-acting glass hydrophobizing agent of the present invention is prepared according to following formula and ratio:
Preparation method:
A) in 77g Virahol, slowly add 3g hydrochloric acid, stir 30min.
B) in a) step solution, slowly add 20g polysiloxane while stirring, continue to stir 8h in room temperature, just can obtain required long-acting glass hydrophobizing agent.
Embodiment six
Long-acting glass hydrophobizing agent of the present invention is prepared according to following formula and ratio:
Preparation method:
A) in the mixing solutions of 80g propyl carbinol, 15g ethanol and 2g water, slowly add 0.5g nitric acid, after stirring 30min, slowly add 2g sulfuric acid again, continue to stir 30min.
B) in a) step solution, slowly add 0.5g polysiloxane, be cooled to room temperature after continuing to stir 12h at 60 DEG C, just can obtain required long-acting glass hydrophobizing agent.
Embodiment seven:
Long-acting glass hydrophobizing agent of the present invention is prepared according to following formula and ratio:
Preparation method:
A) in the mixing solutions of 70g isopropylcarbinol, 25g ethanol and 3g acetonitrile, slowly add 0.5g nitric acid, stir 30min.
B) in a) step solution, slowly add 1.5g polysiloxane, be cooled to room temperature after continuing to stir 6h at 40 DEG C, just can obtain required long-acting glass hydrophobizing agent.
Embodiment eight:
Long-acting glass hydrophobizing agent of the present invention is prepared according to following formula and ratio:
Preparation method:
A) in 90g dehydrated alcohol, slowly add 1g acetic acid, stir 30min.
B) in a) step solution, slowly add 6g polysiloxane 1 while stirring, be placed in 50 DEG C stir 4h after be cooled to room temperature.
C) in above solution, slowly add 3g polysiloxane 2 while stirring, room temperature continues to stir 1h, just can obtain required long-acting glass hydrophobizing agent in batches.
Embodiment nine:
Long-acting glass hydrophobizing agent of the present invention is prepared according to following formula and ratio:
Preparation method:
A) in 9g methyl alcohol and 84g dehydrated alcohol mixed solution, slowly add 1g sulfuric acid, stir 30min.
B) in a) step solution, slowly add 4.5g polysiloxane 1 while stirring, at room temperature stir 10h.
C) in above solution, slowly add 1.5g polysiloxane 2 while stirring, room temperature continues to stir 3h, just can obtain required long-acting glass hydrophobizing agent in batches.
Embodiment ten:
Long-acting glass hydrophobizing agent of the present invention is prepared according to following formula and ratio:
Preparation method:
A) in 80g Virahol, slowly add 2g nitric acid, stir 30min.
B) in a) step solution, slowly add 13g polysiloxane 1 while stirring, stir 5h at 50 DEG C after, be down to room temperature.
C) in b) step solution, slowly add 5g polysiloxane 2 while stirring, room temperature continues to stir 5h, just can obtain required long-acting glass hydrophobizing agent in batches.
Embodiment 11:
Long-acting glass hydrophobizing agent of the present invention is prepared according to following formula and ratio:
Preparation method:
A) slowly add 2g sulfuric acid to limit stirring in 21g dehydrated alcohol and 7g Virahol mixed solution, stir 30min.
B) separately get 60g dehydrated alcohol, add 6g polysiloxane 1 and 3g polysiloxane 3 mixes, after back flow reaction 12h, be cooled to room temperature.
C) in b) step solution, slowly add a) step solution while stirring, continue to stir 30min.
D) in above solution, slowly add 2g polysiloxane 2 while stirring, room temperature continues to stir 1h, just can obtain required long-acting glass hydrophobizing agent in batches.
Embodiment 12
Long-acting glass hydrophobizing agent of the present invention is prepared according to following formula and ratio:
Preparation method:
A) in 92g ethanol, slowly add 2g sulfuric acid, stir 30min.
B) in a) step solution, slowly add 6g methoxy group polysiloxane while stirring, be down to room temperature stir 5h at 50 DEG C after, just can obtain required long-acting glass hydrophobizing agent.
Embodiment 13
Long-acting glass hydrophobizing agent of the present invention is prepared according to following formula and ratio:
Preparation method:
A) in 84.4g propyl carbinol, slowly add 0.6g acetic acid, stir 30min.
B) in a) step solution, slowly add the amino-terminated polymethyl siloxane of 15g while stirring, be down to room temperature stir 5h at 30 DEG C after, just can obtain required long-acting glass hydrophobizing agent.
Using method embodiment:
By long-acting glass hydrophobizing agent obtained for above-described embodiment one to ten three, be applied to glass surface hydrophobic treatment.
Concrete operation method is:
Step 1: by glass surface scrub;
Step 2: glass hydrophobizing agent obtained for embodiment four is coated in glass surface, at room temperature standing waiting until is dried for white film;
Step 3: with clean cotton rub wipe be polished to transparent and bright and clean seamless.
In order to confirm the hydrophobic effect of long-acting glass hydrophobizing agent of the present invention further, the static contact angle of the present invention to the glass surface after hydrophobic treatment and surface of ordinary glass has carried out the hydrophobic effect measuring to judge long-acting glass hydrophobizing agent of the present invention.
In addition, in order to confirm that long-acting glass hydrophobizing agent of the present invention has excellent weather resistance further, simulate issuable loss in actual use procedure by carrying out circulation frictional experiment to the common glass sheet through process of the present invention, the sheet glass of certain brand glass hydrophobizing agent process commercially available of simultaneously learning from else's experience as a comparison.The power that sheet rubber applies 120kPa carries out sliding friction test to sheet glass, and friction frequency is 1 cycle index/second, and a sliding friction is back and forth considered as a cycle index.The abrasive wear resistance of hydrophobic coating is judged by the static contact angle of glass surface to water after measuring different cycle index.
The related data of simple glass in hydrophobicity and wear resistance that table 1 embodiment one to ten three processes
Test result finds: by the long-acting glass hydrophobizing agent of the embodiment of the present invention one to ten three gained for the treatment of glass surface, contact angle before treatment is 13.5 ~ 15.5 °, and the contact angle after process is 101.5 ~ 105.3 °.Such as: simple glass and the glass after the embodiment of the present invention eight processes are contrasted, the data presentation of tested static contact angle, before process, contact angle is 14.7 ± 1.4 °, and is 102.4 ± 1.2 ° (as shown in accompanying drawing 1a-Fig. 1 b) after process.It can thus be appreciated that through the process of gained hydrophobizing agent of the present invention, glass surface all can form effective hydrophobic coating, and water droplet is beaten and naturally tumbled in coating, can not form moisture film at glass surface.
And, judged the abrasive wear resistance of hydrophobic coating by the static contact angle of glass surface to water after measuring different cycle index, result shows that the coating that New-type long-acting glass hydrophobizing agent that the embodiment of the present invention one to ten three obtains is coated on glass surface has higher abrasive wear resistance.Such as, the static contact angle of the circulation rub(bing)test of simple glass after embodiment eight and the process of available glass hydrophobizing agent as shown in Figure 3.Solid dot curve is the glass contact angle through process of the present invention, and after repeatedly rub cycle, contact angle changes hardly as seen; And hollow dots curve is control group, reduce nearly 20% at its contact angle after 1000 rub cycle, illustrate that its surface water-repellent layer has larger wearing and tearing.Here it is pointed out that in testing applied pressure far away higher than vehicle wiper to the issuable actual frictional force of front screen, this is enough to illustrate that above-mentioned coating has sufficiently high abrasive wear resistance.
Secondly, about glass transmission before and after process, the glass that the embodiment of the present invention of learning from else's experience to ten three processes carries out transmittance and compares, and result shows: long-acting glass hydrophobizing agent of the present invention does not affect glass quality, also can not produce any impact (as reflective, smudgy etc.) to sight line.As accompanying drawing 2 be simple glass through before the embodiment of the present invention eight processes (Fig. 2 a) after (Fig. 2 b) light transmittance curve, both before and after visible process, transmittance does not have considerable change, and in visible wavelength range iuuminting rate all more than 95%, to illustrate through this product treatment bare glass light transmission without any impact.
In addition, the glass that the embodiment of the present invention of learning from else's experience to ten three processes is placed in outdoor environment, its surface contact angle of Timing measurement, and result shows, does not substantially change when after six months, its contact angle is compared initial.Such as accompanying drawing 4 represent be through embodiment eight process after sheet glass be placed in outdoor environment different time test static contact angle, contact angle almost keeps constant this product of explanation to have good weather resistance.
Therefore, the long-acting glass hydrophobizing agent obtained by embodiment can with glass surface by chemical bonds, and act synergistically with the inherent nature of macromolecule polysiloxane and form the protective membrane of mortise, hydrophobic effect is lasting.Rainproof, oil-stain-preventing, anti-winter rain, anti-frost can be played, and significantly play self-cleaning action.Contact angle obviously increases and is conducive to water droplet and naturally tumbles and do not adhere to, thus plays waterproof action.Meanwhile, this product does not affect glass quality, can not produce any disadvantageous effect (as reflective, smudgy etc.) to sight line.
It is pointed out that above embodiment and preparation and application to be only used to principle of the present invention is described and the exemplary illustration adopted, 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 (10)
1. a long-acting glass hydrophobizing agent, is characterized in that, be made up of by weight percentage following compositions:
Macromolecule polysiloxane is 0.5 ~ 20wt%;
An acidic catalyst is 0.5 ~ 3wt%;
Solvent 77 ~ 98wt%.
2. long-acting glass hydrophobizing agent according to claim 1, is characterized in that, described macromolecule polysiloxane and an acidic catalyst weight ratio are 3:1 ~ 25:1, account for 2% ~ 15% of gross weight altogether.
3. long-acting glass hydrophobizing agent according to claim 1 and 2, is characterized in that, described macromolecule polysiloxane is one or more that molecular chain-end has the polysiloxane of active function groups end-blocking.
4. long-acting glass hydrophobizing agent according to claim 3, is characterized in that, described active function groups be selected from alkoxyl group, amino, hydroxyl, sulfydryl, chlorine substituent, bromine substituent, epoxy group(ing) one or more.
5. the long-acting glass hydrophobizing agent according to claim arbitrary in Claims 1-4, it is characterized in that, described macromolecule polysiloxane be molecular chain-end there is active function groups end-blocking there are one or more of the long-chain siloxane polymer of certain branched structure, its structural formula general formula can be expressed as:
Wherein x value is 6 ~ 40, y value be 5 ~ 20, z value be 5 ~ 30, n value is 0 ~ 8; R
1, R
2, R
3for active function groups, be selected from the one in alkoxyl group, amino, hydroxyl, sulfydryl, chlorine substituent, bromine substituent, epoxy group(ing), can identical also can be different.
6. long-acting glass hydrophobizing agent according to claim 1, is characterized in that, described an acidic catalyst is one or more in acetic acid, hydrochloric acid, nitric acid, sulfuric acid.
7. long-acting glass hydrophobizing agent according to claim 1, is characterized in that, described solvent is one or more in water, acetonitrile, acetone, methyl alcohol, ethanol, Virahol, propyl carbinol, isopropylcarbinol.
8. the preparation method of the long-acting glass hydrophobizing agent in claim 1 to 7 described in arbitrary claim, is characterized in that, comprising:
Step 1: an acidic catalyst and solvent are obtained acidic medium;
Step 2: add described polysiloxane hybrid reaction in described acidic medium, obtained described long-acting glass hydrophobizing agent.
9. preparation method according to claim 8, is characterized in that, described temperature of reaction is-10-80 DEG C, and the described reaction times is 1-24h.
10. the using method of the long-acting glass hydrophobizing agent in claim 1 to 7 described in arbitrary claim, is characterized in that, comprising:
Step 1: by glass surface scrub;
Step 2: hydrophobizing agent is evenly coated in glass surface, at room temperature leaves standstill and waits until to dry and occur white film;
Step 3: with clean cotton cleaning glass window surface, be polished to bright and clean seamless.
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| CN109678359A (en) * | 2019-01-11 | 2019-04-26 | 湖北新四海化工股份有限公司 | A kind of preparation method and application of self-cleaning glass hydrophobing agent |
| CN109678356A (en) * | 2019-01-11 | 2019-04-26 | 湖北新四海化工股份有限公司 | A kind of high light transmission glass hydrophobing agent and preparation method thereof |
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| CN109678356A (en) * | 2019-01-11 | 2019-04-26 | 湖北新四海化工股份有限公司 | A kind of high light transmission glass hydrophobing agent and preparation method thereof |
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