CN109251612A - A kind of organosilicon water paint and preparation method thereof - Google Patents
A kind of organosilicon water paint and preparation method thereof Download PDFInfo
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- CN109251612A CN109251612A CN201810836529.5A CN201810836529A CN109251612A CN 109251612 A CN109251612 A CN 109251612A CN 201810836529 A CN201810836529 A CN 201810836529A CN 109251612 A CN109251612 A CN 109251612A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
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Abstract
The invention discloses a kind of organosilicon water paint and preparation method thereof, organosilicon water paint includes the component of following parts by weight: 50-80 parts of modified hydroxyl acrylic resin, 45-60 parts of fluorinated polysiloxane, 1-2 parts of initiator, 20-30 parts of organic solvent, 1-5 parts of auxiliary agent.The application is using modified hydroxyl acrylic resin as hydrophilic main even section, by being crosslinking in fluorinated polysiloxane as reaction composition on the hydrophilic main even side chain of section of modified hydroxyl acrylic resin, after the paint film that paint solidification is formed, fluorinated polysiloxane connects section as organosilicon, due to the constraint being less subject in structure, it can be with free extension, therefore the micro molecule layer of higher fluorinated polysiloxane density can be formed in film coated surface, therefore the surface of the paint film structure that paint solidification is formed is fine and close enough, to assign film coated surface very good antigraffiti effect.
Description
Technical field
The present invention relates to a kind of water paint technologies more particularly to a kind of organosilicon water paint and preparation method thereof.
Background technique
As living standard is continuously improved, people are also increasingly strict to the requirement of building coating.Traditional inorganic dress
Exterior material extremely difficult cleaning after metope is scribbled or made dirty when building wall makees facing.Scientific research personnel is in anti-doodling and anti-affixing coating
Research and development on a few thing has also been made, the study found that organosilicon auxiliary agent have excellent hydrophobic and lyophobic property and lubricity,
It is applied in coating, the surface energy of film can be significantly reduced, obtain splendid low-surface-energy effect.
But in existing anti-graffiti and anti-pollution water paint, effective ingredient is only in the surface of the paint film of paint solidification formation
Upper addition organosilicon auxiliary agent, but its additive amount is few, silicone segments are often in the position of main chain, final coating film with
Afterwards, silicone segments are often arranged in film coated surface, but are limited by its structure, are often unable to fully trail, and office
Limit in a certain range, therefore can only assign film corresponding slippery, be unable to reach the close of anti-graffiti required silicone segments
Degree.Therefore, scribble substance and stain easily penetrates among paint film and causes not easy to clean, and this surface of the paint film is passed through and repeatedly wiped
It washes rear such active principle to be easy to wear, thus will lead to its anti-graffiti and stain resistance and weaken, reduced service life, again
The problems such as coating is again difficult.
Summary of the invention
For overcome the deficiencies in the prior art, one of the objects of the present invention is to provide a kind of organosilicon water paints.This
Application is changed using modified hydroxyl acrylic resin as hydrophilic main even section by the way that fluorinated polysiloxane to be crosslinking in as reaction composition
Property Hydroxylated acrylic resin it is hydrophilic it is main even section side chain on, paint solidification formed paint film after, fluorinated polysiloxane is as organic
Silicon connects section, due to the constraint being less subject in structure, can be formed in film coated surface higher fluorine-containing poly- with free extension
The micro molecule layer of siloxanes density, therefore the surface of the paint film structure that paint solidification is formed is fine and close enough, to assign film table
The very good antigraffiti effect in face.
The second object of the present invention is to provide a kind of preparation method of organosilicon water paint.Preparation method is simple, system
Standby mild condition, reproducible, yield is high, has broad application prospects.
An object of the present invention adopts the following technical scheme that realization: a kind of organosilicon water paint, including following weight
The component of number: 50-80 parts of modified hydroxyl acrylic resin, 45-60 parts of fluorinated polysiloxane, 1-2 parts of initiator, organic solvent
20-30 parts, 1-5 parts of auxiliary agent.
Further, the modified hydroxyl acrylic resin is value for 80-150mgKOH/g, and number-average molecular weight is
2000-20000g/mol。
Further, the fluorinated polysiloxane is prepared by following component: 50 parts by weight of fluorosilicon oil, silane 8-15 weight
Measure part, catalyst 10-100ppm, solvent 10-30 parts by weight.
Further, the silane is trimethoxy silane, triethoxysilane, vinyltrimethoxysilane, ethylene
One of ethyl triethoxy silicane alkane, acryloxy trimethoxy silane, acryloxy triethoxysilane；Catalyst is
One of Speier catalyst, Karstedt catalyst；The solvent is one of THF, toluene, DMF.
Further, the fluorinated polysiloxane the preparation method is as follows: first reaction unit is vacuumized, keep vacuum degree
It is 1.5 × 10-1pa；Oxygen and moisture are removed, then is passed through nitrogen protection；Be added 50 parts by weight of fluorosilicon oil, silane 8-15 parts by weight,
Catalyst 10-100ppm, solvent 10-30 parts by weight, stir evenly；Reaction 2-5 hours is carried out at 65-75 DEG C；Product transfer
Into decompression rotary evaporator, 1.5 × 10-1Under pa vacuum degree, revolving 30min is carried out at 20-50 DEG C to get fluorine-containing poly- silicon
Oxygen alkane.
Further, the initiator is one or more of azo-initiator, peroxide initiator；The idol
Nitrogen class initiator is the mixture of one or both of azodiisobutyronitrile, azobisisoheptonitrile；The peroxide initiator is
One of dibenzoyl peroxide, di-t-butyl peroxide, di t-amyl peroxide.
Further, the organic solvent is propylene glycol, in ether, acetate, n-butanol, dimethylbenzene, butyl acetate
One or more kinds of mixtures.
Further, the auxiliary agent is coalescing agent, levelling agent, antifreezing agent, defoaming agent, thickener, one in mould inhibitor
Kind or two or more mixtures.
The second object of the present invention adopts the following technical scheme that realization: a kind of preparation method of organosilicon water paint, packet
Include following steps:
(1) organic solvent is added in the four-hole boiling flask equipped with agitating paddle, thermometer and condenser pipe, is warming up to 100-160
℃；
(2) modified hydroxyl acrylic resin and initiator are mixed, stirring makes to be uniformly mixed, and forms part A；
(3) fluorinated polysiloxane is stirred, makes to be uniformly mixed, forms part B；
(4) part B is added in flask, part A is packed into Dropping feeder, be added dropwise in 2-5 hours with constant speed；It drips
Temperature is increased 5-10 DEG C and keeps the temperature 2 hours by Bi Hou；
(5) temperature is reduced to 70 DEG C and hereinafter, auxiliary agent is added, and stirring discharges after 10-30 minutes.
Further, the fluorine polysiloxanes the preparation method is as follows: first reaction unit is vacuumized, keep the vacuum degree to be
1.5×10-1pa；Oxygen and moisture are removed, then is passed through nitrogen protection；50 parts of fluorosilicon oil, 8-15 parts of silane, catalyst 10- is added
10-30 parts of 100ppm, solvent, stir evenly；Reaction 2-5 hours is carried out at 65-75 DEG C；Product is transferred to decompression rotary evaporation
In device, 1.5 × 10-1Under pa vacuum degree, revolving 30min is carried out at 20-50 DEG C to get fluorinated polysiloxane.
Compared with prior art, the beneficial effects of the present invention are:
(1) the application is using modified hydroxyl acrylic resin as hydrophilic main even section, by using fluorinated polysiloxane as anti-
Composition is answered to be crosslinking on the hydrophilic main even side chain of section of modified hydroxyl acrylic resin, it is fluorine-containing poly- after the paint film that paint solidification is formed
Siloxanes connects section as organosilicon, can be with free extension due to the constraint being less subject in structure, therefore can be in film coated surface shape
At the micro molecule layer of higher fluorinated polysiloxane density, therefore the surface of the paint film structure that paint solidification is formed is fine and close enough,
To assign film coated surface very good antigraffiti effect.
(2) backbone structure of the fluorinated polysiloxane of the application is submissive organosilicon chain, introduces property on side chain and stablizes
And the extremely low organic fluorine chain of surface tension make it have lower surface can, the performance of smoothness and oil resistant.The fluorine-containing poly- silicon
Oxygen alkane further improves the oil repellency of water paint.
(3) preparation method of the present invention is simple, and preparation condition is mild, reproducible, and yield is high, before wide application
Scape.
Specific embodiment
In the following, being described further in conjunction with specific embodiment to the present invention, it should be noted that is do not collided
Under the premise of, new embodiment can be formed between various embodiments described below or between each technical characteristic in any combination.
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, used equipment and raw material etc.
It is commercially available or commonly used in the art.Method in following embodiments is unless otherwise instructed the normal of this field
Rule method.
A kind of organosilicon water paint, the component including following parts by weight: 50-80 parts of modified hydroxyl acrylic resin,
45-60 parts of fluorinated polysiloxane, 1-2 parts of initiator, 20-30 parts of organic solvent, 1-5 parts of auxiliary agent.
Further, the modified hydroxyl acrylic resin is value for 80-150mgKOH/g, and number-average molecular weight is
2000-20000g/mol。
Further, the fluorinated polysiloxane is prepared by following component: 50 parts by weight of fluorosilicon oil, silane 8-15 weight
Measure part, catalyst 10-100ppm, solvent 10-30 parts by weight.
Further, the silane is trimethoxy silane, triethoxysilane, vinyltrimethoxysilane, ethylene
One of ethyl triethoxy silicane alkane, acryloxy trimethoxy silane, acryloxy triethoxysilane；Catalyst is
One of Speier catalyst, Karstedt catalyst；The solvent is one of THF, toluene, DMF.
Further, the fluorinated polysiloxane the preparation method is as follows: first reaction unit is vacuumized, keep vacuum degree
It is 1.5 × 10-1pa；Oxygen and moisture are removed, then is passed through nitrogen protection；Be added 50 parts by weight of fluorosilicon oil, silane 8-15 parts by weight,
Catalyst 10-100ppm, solvent 10-30 parts by weight, stir evenly；Reaction 2-5 hours is carried out at 65-75 DEG C；Product transfer
Into decompression rotary evaporator, 1.5 × 10-1Under pa vacuum degree, revolving 30min is carried out at 20-50 DEG C to get fluorine-containing poly- silicon
Oxygen alkane.
Further, the initiator is one or more of azo-initiator, peroxide initiator；The idol
Nitrogen class initiator is the mixture of one or both of azodiisobutyronitrile, azobisisoheptonitrile；The peroxide initiator is
One of dibenzoyl peroxide, di-t-butyl peroxide, di t-amyl peroxide.
Further, the organic solvent is propylene glycol, in ether, acetate, n-butanol, dimethylbenzene, butyl acetate
One or more kinds of mixtures.
Further, the auxiliary agent is coalescing agent, levelling agent, antifreezing agent, defoaming agent, thickener, one in mould inhibitor
Kind or two or more mixtures.The coalescing agent is 2,2,4- trimethyl -1,3- pentanediol-isobutyl acid monoester；State levelling
Agent is esters of acrylic acid levelling agent, silicone polyether acrylate class levelling agent or polyethers silicon oxygen Anhui class levelling agent；It is described antifreeze
Agent is ethylene glycol；The defoaming agent is mineral oil defoaming agent, the model CF245 produced with England Blackburn chemical company
Defoaming agent；The thickener is alkali-swelling type thickener, with the thickener for the model TT935 that Dow Chemical produces；
The mould inhibitor is OIT class mould inhibitor, the model LXE preservative produced with ROHM AND HAAS China Investment Ltd..
The second object of the present invention adopts the following technical scheme that realization: a kind of preparation method of organosilicon water paint, packet
Include following steps:
(1) organic solvent is added in the four-hole boiling flask equipped with agitating paddle, thermometer and condenser pipe, is warming up to 100-160
℃；
(2) modified hydroxyl acrylic resin and initiator are mixed, stirring makes to be uniformly mixed, and forms part A；
(3) fluorinated polysiloxane is stirred, makes to be uniformly mixed, forms part B；
(4) part B is added in flask, part A is packed into Dropping feeder, be added dropwise in 2-5 hours with constant speed；It drips
Temperature is increased 5-10 DEG C and keeps the temperature 2 hours by Bi Hou；
(5) temperature is reduced to 70 DEG C and hereinafter, auxiliary agent is added, and stirring discharges after 10-30 minutes.
Further, the fluorine polysiloxanes the preparation method is as follows: first reaction unit is vacuumized, keep the vacuum degree to be
1.5×10-1pa；Oxygen and moisture are removed, then is passed through nitrogen protection；50 parts of fluorosilicon oil, 8-15 parts of silane, catalyst 10- is added
10-30 parts of 100ppm, solvent, stir evenly；Reaction 2-5 hours is carried out at 65-75 DEG C；Product is transferred to decompression rotary evaporation
In device, 1.5 × 10-1Under pa vacuum degree, revolving 30min is carried out at 20-50 DEG C to get fluorinated polysiloxane.
Embodiment 1-5
The proportion according to the form below 1 weighs raw material respectively, is prepared as steps described below, the difference is that added
Raw material proportioning is different, prepares product, and specific see Table 1 for details:
Table 1: embodiment 1-5 raw material proportioning table
Wherein, the modified hydroxyl acrylic resin be value be 80-150mgKOH/g, number-average molecular weight 2000-
20000g/mol。
Fluorinated polysiloxane the preparation method is as follows: first reaction unit is vacuumized, keeping vacuum degree is 1.5 × 10-1pa；
Oxygen and moisture are removed, then is passed through nitrogen protection；50 parts by weight of fluorosilicon oil, 10 parts by weight of trimethoxy silane, Speier are added
Catalyst 50ppm, 20 parts by weight of toluene, stir evenly；Reaction 3 hours is carried out at 70 DEG C；Product is transferred to decompression rotation and steams
It sends out in device, 1.5 × 10-1Under pa vacuum degree, revolving 30min is carried out at 35 DEG C to get fluorinated polysiloxane.
Initiator is azodiisobutyronitrile.Organic solvent is with propylene glycol.Auxiliary agent is the defoaming agent of CF245.
The preparation method of the organosilicon water paint of embodiment 1-5, includes the following steps:
(1) organic solvent is added in the four-hole boiling flask equipped with agitating paddle, thermometer and condenser pipe, is warming up to 120 DEG C；
(2) modified hydroxyl acrylic resin and initiator are mixed, stirring makes to be uniformly mixed, and forms part A；
(3) fluorinated polysiloxane is stirred, makes to be uniformly mixed, forms part B；
(4) part B is added in flask, part A is packed into Dropping feeder, is added dropwise in 3 hours with constant speed；It is added dropwise
Afterwards, temperature is increased 8 DEG C and keeps the temperature 2 hours；
(5) temperature is reduced to 70 DEG C and hereinafter, auxiliary agent is added, and stirring discharges after twenty minutes.
The coating of above-described embodiment is sprayed on defined various substrates, after paint film is fully cured on substrate, root
Properties test is carried out according to the requirement of technical performance result, comprising: appearance, salt fog resistance, artificial ageing resistance, is prevented at wearability
Scribble property, specific test performance result see the table below 2:
The results of property of 2 embodiment 1-5 of table
Water paint of the invention not only has excellent anti-graffiti property, in addition, wearability, salt spray resistance, artificial ageing resistance
Performance is prominent.
The above embodiment is only the preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto,
The variation and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed range.
Claims (10)
1. a kind of organosilicon water paint, which is characterized in that the component including following parts by weight: modified hydroxyl acrylic resin
50-80 parts, 45-60 parts of fluorinated polysiloxane, 1-2 parts of initiator, 20-30 parts of organic solvent, 1-5 parts of auxiliary agent.
2. organosilicon water paint as described in claim 1, which is characterized in that the modified hydroxyl acrylic resin is value
For 80-150mgKOH/g, number-average molecular weight 2000-20000g/mol.
3. organosilicon water paint as described in claim 1, which is characterized in that the fluorinated polysiloxane is by following component system
It is standby to form: 50 parts by weight of fluorosilicon oil, silane 8-15 parts by weight, catalyst 10-100ppm, solvent 10-30 parts by weight.
4. organosilicon water paint as claimed in claim 3, which is characterized in that the silane is trimethoxy silane, three second
Oxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, acryloxy trimethoxy silane, acryloyl
One of oxygroup triethoxysilane；Catalyst is one of Speier catalyst, Karstedt catalyst；The solvent
For one of THF, toluene, DMF.
5. organosilicon water paint as described in claim 1, which is characterized in that the preparation method of the fluorinated polysiloxane is such as
Under: first reaction unit is vacuumized, keeping vacuum degree is 1.5 × 10-1pa；Oxygen and moisture are removed, then is passed through nitrogen protection；Add
Enter 50 parts by weight of fluorosilicon oil, silane 8-15 parts by weight, catalyst 10-100ppm, solvent 10-30 parts by weight, stirs evenly；?
Reaction 2-5 hours is carried out at 65-75 DEG C；Product is transferred in decompression rotary evaporator, 1.5 × 10-1Under pa vacuum degree,
Revolving 30min is carried out at 20-50 DEG C to get fluorinated polysiloxane.
6. organosilicon water paint as described in claim 1, which is characterized in that the initiator is azo-initiator, mistake
One or more of oxygen class initiator；The azo-initiator is azodiisobutyronitrile, one in azobisisoheptonitrile
Kind or two kinds of mixture；The peroxide initiator is dibenzoyl peroxide, di-t-butyl peroxide, di t-amyl peroxide
One of.
7. organosilicon water paint as described in claim 1, which is characterized in that the organic solvent is propylene glycol, ether, vinegar
The mixture of one or more of acid esters, n-butanol, dimethylbenzene, butyl acetate.
8. organosilicon water paint as described in claim 1, which is characterized in that the auxiliary agent is coalescing agent, levelling agent, prevents
Freeze the mixture of one or more of agent, defoaming agent, thickener, mould inhibitor.
9. a kind of preparation method of organosilicon water paint, which comprises the steps of:
(1) organic solvent is added in the four-hole boiling flask equipped with agitating paddle, thermometer and condenser pipe, is warming up to 100-160 DEG C；
(2) modified hydroxyl acrylic resin and initiator are mixed, stirring makes to be uniformly mixed, and forms part A；
(3) fluorinated polysiloxane is stirred, makes to be uniformly mixed, forms part B；
(4) part B is added in flask, part A is packed into Dropping feeder, be added dropwise in 2-5 hours with constant speed；It is added dropwise
Afterwards, temperature is increased 5-10 DEG C and keeps the temperature 2 hours；
(5) temperature is reduced to 70 DEG C and hereinafter, auxiliary agent is added, and stirring discharges after 10-30 minutes.
10. preparation method as claimed in claim 9, which is characterized in that the fluorine polysiloxanes the preparation method is as follows: first will
Reaction unit vacuumizes, and keeping vacuum degree is 1.5 × 10-1pa；Oxygen and moisture are removed, then is passed through nitrogen protection；Fluorine silicon is added
Oily 50 parts, 8-15 parts of silane, catalyst 10-100ppm, 10-30 parts of solvent, stir evenly；Reaction 2-5 is carried out at 65-75 DEG C
Hour；Product is transferred in decompression rotary evaporator, 1.5 × 10-1Under pa vacuum degree, rotated at 20-50 DEG C
30min is to get fluorinated polysiloxane.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810836529.5A CN109251612B (en) | 2018-07-26 | 2018-07-26 | Organic silicon water-based paint and preparation method thereof |
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| CN201810836529.5A CN109251612B (en) | 2018-07-26 | 2018-07-26 | Organic silicon water-based paint and preparation method thereof |
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| CN109251612B CN109251612B (en) | 2021-11-19 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110484136A (en) * | 2019-08-26 | 2019-11-22 | 湖南辰砾新材料有限公司 | A kind of waterborne organic silicon coating and preparation method thereof |
| CN111777910A (en) * | 2020-07-28 | 2020-10-16 | 天津中航百慕新材料技术有限公司 | Water-based graphite allyl acid-polysiloxane coating and preparation method thereof |
| CN115304980A (en) * | 2022-09-01 | 2022-11-08 | 瑞悦汽车工业(重庆)有限公司 | Surface treatment process for processing automobile bumper strip |
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| CN111777910A (en) * | 2020-07-28 | 2020-10-16 | 天津中航百慕新材料技术有限公司 | Water-based graphite allyl acid-polysiloxane coating and preparation method thereof |
| CN115304980A (en) * | 2022-09-01 | 2022-11-08 | 瑞悦汽车工业(重庆)有限公司 | Surface treatment process for processing automobile bumper strip |
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| CN109251612B (en) | 2021-11-19 |
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