CN108893051B - A kind of preparation method and applications for the organosilane polymer coating material coating hydrophobic powder layer by layer - Google Patents

A kind of preparation method and applications for the organosilane polymer coating material coating hydrophobic powder layer by layer Download PDF

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CN108893051B
CN108893051B CN201810449982.0A CN201810449982A CN108893051B CN 108893051 B CN108893051 B CN 108893051B CN 201810449982 A CN201810449982 A CN 201810449982A CN 108893051 B CN108893051 B CN 108893051B
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layer
coating
hydrophobic powder
polymer
organosilane polymer
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CN108893051A (en
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吴磊
张想泰
谢子康
司杨
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Qinghai University
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Qinghai University
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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
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/36—After-treatment
    • C08J9/365—Coating
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention discloses a kind of preparation method and applications of organosilane polymer coating material for coating hydrophobic powder layer by layer, belong to special wetability coating material field.The material is that hydrophobic powder is effectively coated with ethyl orthosilicate, then using two kinds of organosilans of ethyl orthosilicate and hexadecyl trimethoxy silane as presoma, hydrolytic condensation and obtain.Have the characteristics that preparation method is simple, property is stable, good waterproof performance.Coating material has the excellent characteristics such as low surface tension, high-low temperature resistant, good weatherability, is widely used in the industries such as building and weave.

Description

A kind of preparation method for the organosilane polymer coating material coating hydrophobic powder layer by layer And its application
Technical field
The invention belongs to coating material technical fields, are related to a kind of system for coating organosilane polymer coating material layer by layer Preparation Method；The invention further relates to application of the organosilane polymer coating material in waterproofing agent.
Background technique
Impervious, waterproof and leak repairing are always always architectural engineering industry one the problem of being concerned.People develop thus Various waterproofing agents, impervious additive and water-repellent paint.Although traditional pitch craft leakage mending method can play the role of water proof anti-seepage, But based on its higher cost, difficulty of construction is big, by ultraviolet light influenced with validity period it is shorter the problems such as and by denouncing.With excellent Different waterproof performance, resistant to chemical etching, efflorescence prevention and it is anti-peel off etc. performances waterproofing agent of organosilicon in buildings waterproof industry take off grain husk and Out, it and is used widely.Waterproofing agent of organosilicon is reacted with the hydroxyl in cement mortar, is combined into network structure.Cement mortar After solidification, the hydrophobic grouping in organosilicon reduces the surface energy of material surface, the intrusion of water is prevented, to reduce cement mortar Water absorption rate maintains the self performance of cement mortar well.The active component that common are machine silicon waterproofing agent in the market is main It is organosilicate, silane, siloxanes and silicone resin etc..Waterproof is constructed in combination usually according to both roughness and low-surface-energy Surface, the existing method for preparing water-proof surface and type are very much, but existing preparation method excessively relies on complicated chemicals Matter and accurate experimental facilities.Secondly, generally using fluorine-containing or silane compound as low-surface energy substance, it is expensive and Environmental hazard is big.Meanwhile longer manufacturing cycle is also the problem currently faced, these there are the problem of result in difficulty To be effectively prepared the water-proof surface of large area.Based on this, using the microstructure of simple effective method structured surface, thus Consistency of performance and excellent water-proof surface are obtained, and the various aspects for being efficiently applied to actual production and daily life are to be badly in need of solution Certainly the problem of.
Summary of the invention
In order to overcome the above-mentioned problems in the prior art, present invention aims at the hydrolytic condensations using organosilan Reaction provides a kind of preparation method of organosilane polymer coating material for coating hydrophobic powder layer by layer.
To achieve the goals above, The technical solution adopted by the invention is as follows: a kind of organosilicon for coating hydrophobic powder layer by layer The preparation method of alkane polymer coating materials is with ethyl orthosilicate (TEOS) effectively cladding hydrophobic powder (WA), then with positive silicic acid Two kinds of organosilans of ethyl ester (TEOS) and hexadecyl trimethoxy silane (HDTMS) are presoma, and hydrolytic condensation is up to layer by layer Coat the organosilane polymer coating material of hydrophobic powder；Specifically includes the following steps:
Hydrophobic powder (WA) and ethyl orthosilicate (TEOS) are dissolved in ethyl alcohol and ammonia-alcohol mixed solvent first by step A. In, it stirs 0.5 hour, makes to be uniformly mixed, 80 °C are after the reaction was completed, filter, and the hydrophobic powder of coated with silica is obtained after dry Grain WA@SiO2；
Step B. is again by the obtained product of step A and ethyl orthosilicate (TEOS) and hexadecyl trimethoxy silane (HDTMS) both organosilans are dissolved in ethyl alcohol and ammonia-alcohol mixed solvent, are stirred 0.5 hour, are made to be uniformly mixed, 80 °C after the reaction was completed, it filters, is coated the organosilane polymer WA@SiO of hydrophobic powder after dry layer by layer2@HD-silica/ HD-polymer。
A kind of organosilane polymer coating material of hydrophobic powder that coats layer by layer of the above-mentioned preparation of the present invention is as special profit Application of the moist coating in waterproofing agent.
The organosilane polymer coating material for coating hydrophobic powder layer by layer of the above-mentioned preparation of the present invention is by being simply coated with Method constructs waterproof coating on sponge base material, realizes the application in waterproofing agent.
The above-mentioned organosilane polymer work for coating hydrophobic powder layer by layer is utilized another object of the present invention is to provide a kind of Simple dip coating is utilized for coating material, the lasting excellent polymer coating with fire resistance characteristic of structural behavior uses Technical solution is in this way: using sponge as coating substrate material, taking organosilane polymer made from 40 mg step B to take and 10 mL are added In toluene, concussion is dispersed in polymer in toluene, is coated on sponge surface using dip coating, obtains with fire resistance characteristic Polymer coating.Functional group (hydroxyl) abundant is formed new in conjunction with the silicone hydroxyl of polymer surfaces on sponge base material Silicon oxygen silicon key, ultimately forms stable waterproof coating.
To the present invention have fire resistance characteristic layer by layer coat hydrophobic powder organosilane polymer coating material performance into Row test and evaluation.
Fig. 1 is coated with silica hydrophobic powder WA@SiO2(a1 and a2) and gathered again with what two kinds of organosilans coated Close object WA@SiO2@HD-silica/HD-polymer (b1 and b2) transmission electron microscope picture.Pass through titanium dioxide as seen in Figure 1 Hydrophobic powder ball after silicon cladding is poly- more severe, goes out spherical particle in the edge observable of the transmission electron microscope photo (a2) of amplification Presence.With gathering after two kinds of organosilan claddings of ethyl orthosilicate (TEOS) and hexadecyl trimethoxy silane (HDTMS) Close object WA@SiO2The agglomeration of@HD-silica/HD-polymer particle be improved significantly (figure b2).From electromicroscopic photograph It can be seen that the size of hydrophobic powder particles is 200 nm, indicated with virtual coil A.The presentation of coated with silica hydrophobic powder is spherical, Particle size is about 500 nm, is indicated with virtual coil B.And the diameter of the particle of the polymer of two kinds of organosilans cladding is about 0.8- 1.1 micron.And the polymer WA@SiO coated layer by layer2It is not mutually solely between@HD-silica/HD-polymer ball and ball Vertical, but (white arrow in figure b2) is attached by cetyl-silica/cetyl polymer, illustrate two Polymer after kind organosilan hydrolytic condensation imparts the coarse structure of material nano grade.
Fig. 2 is coated with silica hydrophobic powder WA@SiO2The polymer WA@coated again with two kinds of organosilans SiO2The infrared spectrum of@HD-silica/HD-polymer.After two infrared spectrums compare, it was found that apparent new suction Receive the appearance at peak.It can be seen that the waterproof coating polymer arrived of TEOS and HDTMS under alkaline condition after hydrolytic condensation exists 1082 and 799 cm-1The absorption peak at place is Si-O-Si key asymmetry and symmetrical stretching vibration in polysiloxanes.Illustrate that TEOS is hydrolyzed SiO afterwards2Surface is modified by cetyl, and assigns material low-surface-energy.949 cm-1The absorption peak at place is the deformation of Si-OH Vibration.Infrared spectrum characterization demonstrates ethyl orthosilicate and hexadecyl trimethoxy silane has successfully modified coated with silica Hydrophobic powder particles.
Fig. 3 is the organosilane polymer WA@SiO for coating hydrophobic powder layer by layer2@HD-silica/HD-polymer is same respectively When dispersed photo (5 mg/mL) in five kinds of toluene, n-hexane, methanol, dehydrated alcohol and acetone solvents.Polymer is in first It cannot be completely dissolved in alcohol, dehydrated alcohol and acetone, Cong Tuzhong is it will be clear that white particle will adhere to after concussion In vial inside-wall.And polymer can not be completely dispersed after shaking in n-hexane, bottom of bottle can sedimented particle, only Ultrasonic Heating After could be fully dispersed.Coated polymer WA@SiO layer by layer2@HD-silica/HD-polymer can be completely dispersed in toluene It is even.Toluene is optimum solvent in dispersion stabilization experiment.
Fig. 4 is to coat hydrophobic powder organosilane polymer WA@SiO layer by layer2@HD-silica/HD-polymer is coated on two The water droplet photo before and after coating on kind sponge.Sponge a and b are polyurethane sponge, and sponge a is aperture, and b is closed pore.For Observation is clear, in advance water droplet is dyed (10 ppm MB).Hydrophobic powder is coated from water droplet (7 μ L) in olynthus and layer by layer Organosilane polymer coating sponge on photo in find out, water droplet is adherency first on olynthus surface, after 1 min gradually Wetting, repaves exhibition sponge surface.And be coated with the sponge for coating the organosilane polymer of hydrophobic powder layer by layer, due to roughness and The introducing of low-surface energy substance, shows super-hydrophobicity.This simple dip coating can uniformly be coated on entire sponge Three-dimensional space, it is final to assign material super-hydrophobicity, realize the function of waterproof.
Fig. 5 is 7 μ L water droplets on olynthus and polymer WA@SiO2@HD-silica/HD-polymer coats sponge Contact angle photo.Contact angle of the 7 μ L water droplets on olynthus surface is 85 °, after 1 min, water droplet complete wetting olynthus surface. Since the synergistic effect of roughness and low-surface energy substance makes the sponge surface for being coated with polymer show super-hydrophobicity, cause Water droplet is presented fully spherical shape, assigns material waterproofing performance.
In conclusion the organosilane polymer imparting coating material prepared by the present invention for coating hydrophobic powder layer by layer is lower Surface energy and roughness.Coating surface shows the characteristic of waterproof.It can be on sponge base material by simple rubbing method Waterproof coating is constructed, realizes the application in waterproofing agent.
Compared with prior art, a kind of organosilane polymer coating material coating hydrophobic powder layer by layer provided by the invention Material is hydrophobic powder effectively to be coated with ethyl orthosilicate, then (ethyl orthosilicate coats hydrophobic powder using two kinds of organosilans as presoma It is organosilane-modified with two kinds again afterwards), the organosilan polymerization for coating hydrophobic powder layer by layer is prepared using hydrolysis-condensation reaction Object, the organosilane polymer coating with fire resistance characteristic that can be had excellent performance after simple dip-coating.The present invention Simple with application method, formation coating performance stabilization, good waterproof performance etc. have low surface tension, high-low temperature resistant, weatherability The excellent characteristics such as good can be widely applied for the industries such as building and weave.
Detailed description of the invention
Fig. 1 is coated with silica hydrophobic powder WA@SiO2 (a1 and a2) and the polymer coated again with two kinds of organosilans WA@SiO2The transmission electron microscope picture of@HD-silica/HD-polymer (b1 and b2)；
Fig. 2 is coated with silica hydrophobic powder WA@SiO2The polymer WA@SiO coated again with two kinds of organosilans2@ The infrared spectrum of HD-silica/HD-polymer；
Fig. 3 is the organosilane polymer WA@SiO for coating hydrophobic powder layer by layer2@HD-silica/HD-polymer is in first Benzene, n-hexane, methanol, the dispersed photo (5 mg/mL) in five kinds of solvents of dehydrated alcohol and acetone；
Fig. 4 is the organosilane polymer WA@SiO for coating hydrophobic powder layer by layer2@HD-silica/HD-polymer is coated on The water droplet photo before and after coating on two kinds of sponges；
Fig. 5 is the organosilane polymer WA@SiO that 7 μ L water droplets coat hydrophobic powder on olynthus and layer by layer2@HD- The contact angle photo of silica/HD-polymer coating sponge.
Specific embodiment
The preparation of coating material of the present invention is described further below by specific example, and is with different dispersion solvents Example, illustrates the superiority of polymer coating materials dispersion performance prepared by the present invention.
Embodiment 1
A kind of preparation method for the organosilane polymer coating hydrophobic powder layer by layer, specifically includes the following steps:
Hydrophobic powder (WA) and ethyl orthosilicate (TEOS) are dissolved in ethyl alcohol and ammonia-alcohol mixed solvent by step A., are stirred It mixes 0.5 hour, makes to be uniformly mixed.80 °C after the reaction was completed, filters, and the hydrophobic powder particles of coated with silica are obtained after dry (WA@SiO2).Step B. again by the obtained product of step A and TEOS and hexadecyl trimethoxy silane (HDTMS) both Organosilan is dissolved in EtOH and NH3- EtOH in the mixed solvent stirs 0.5 hour, makes to be uniformly mixed.80 °C of reactions are completed Afterwards, it filters, is coated organosilane polymer (the WA@SiO of hydrophobic powder after dry layer by layer2@HD-silica/HD- Polymer) coating material.
A kind of side prepare using the organosilane polymer for coating hydrophobic powder layer by layer of above-mentioned preparation waterproof coating Method:
Waterproof coating prepared by the present invention is using sponge as coating substrate material, and 10 mL toluene are added in 40 mg polymer In, concussion is dispersed in polymer in toluene, obtains having more superb hydrophobic polymer coating, assigns material waterproofing Performance.
Embodiment 2
A kind of preparation method for the organosilane polymer coating hydrophobic powder layer by layer, specifically includes the following steps:
Hydrophobic powder (WA) and ethyl orthosilicate (TEOS) are dissolved in ethyl alcohol and ammonia-alcohol mixed solvent by step A., are stirred It mixes 0.5 hour, makes to be uniformly mixed.80 °C after the reaction was completed, filters, and the hydrophobic powder particles of coated with silica are obtained after dry (WA@SiO2).Step B. again by the obtained product of step A and TEOS and hexadecyl trimethoxy silane (HDTMS) both Organosilan is dissolved in EtOH and NH3- EtOH in the mixed solvent stirs 0.5 hour, makes to be uniformly mixed.80 °C of reactions are completed Afterwards, it filters, is coated organosilane polymer (the WA@SiO of hydrophobic powder after dry layer by layer2@HD-silica/HD- Polymer) coating material.
A kind of side prepare using the organosilane polymer for coating hydrophobic powder layer by layer of above-mentioned preparation waterproof coating Method:
Waterproof coating prepared by the present invention, be using sponge as coating substrate material, 40 mg polymer be added 10 mL just oneself In alkane, concussion post-consumer polymer cannot be dispersed in n-hexane, remain to see white solid particle.It heats under ultrasound condition Can with dissolution be scattered in n-hexane.By sponge dip-coating on sponge, obtaining that there is hydrophobic polymer coating.
Embodiment 3
A kind of preparation method for the organosilane polymer coating hydrophobic powder layer by layer, specifically includes the following steps:
Hydrophobic powder (WA) and ethyl orthosilicate (TEOS) are dissolved in ethyl alcohol and ammonia-alcohol mixed solvent by step A., are stirred It mixes 0.5 hour, makes to be uniformly mixed, 80 °C after the reaction was completed, filters, and the hydrophobic powder particles of coated with silica are obtained after dry (WA@SiO2).Step B. again by the obtained product of step A and TEOS and hexadecyl trimethoxy silane (HDTMS) both Organosilan is dissolved in EtOH and NH3- EtOH in the mixed solvent stirs 0.5 hour, makes to be uniformly mixed, and 80 °C of reactions are completed Afterwards, it filters, is coated organosilane polymer (the WA@SiO of hydrophobic powder after dry layer by layer2@HD-silica/HD- polymer)。
The method for preparing polymer coating is carried out using the above-mentioned organosilane polymer for coating hydrophobic powder layer by layer:
Polymer coating prepared by the present invention is using sponge as coating substrate material, and 10 mL second are added in 40 mg polymer In alcohol, concussion post-consumer polymer cannot be dispersed in ethyl alcohol, remain to see white solid particle.Under heating ultrasound condition also not It can dissolve and be scattered in ethyl alcohol well.It, also cannot good waterproof without hydrophobic performance after supernatant carries out dip-coating.
The preferred technical grade multi-component copolymer type hydrophobic powder of hydrophobic powder of the present invention, main component are lipid organic products Mixture.

Claims (5)

1. a kind of preparation method for the organosilane polymer coating material for coating hydrophobic powder layer by layer, it is characterised in that: with positive silicon Acetoacetic ester effectively coats hydrophobic powder, then with two kinds of organosilans of ethyl orthosilicate and hexadecyl trimethoxy silane is forerunner Body, hydrolytic condensation coat the organosilane polymer coating material of hydrophobic powder layer by layer to obtain the final product, specifically includes the following steps:
Hydrophobic powder and ethyl orthosilicate are dissolved in ethyl alcohol and ammonia-alcohol mixed solvent by step A. first, and stirring keeps mixing equal Even, heating filters after the reaction was completed, is dry, obtains the hydrophobic powder particles WA@SiO of coated with silica2；
Step B. again by the obtained product of step A and ethyl orthosilicate and hexadecyl trimethoxy silane be dissolved in ethyl alcohol and In ammonia-alcohol mixed solvent, stirring makes to be uniformly mixed, and heating filters after the reaction was completed, drying is to get cladding hydrophobic powder layer by layer Organosilane polymer WA@SiO2@HD-silica/HD-polymer。
2. a kind of preparation method of organosilane polymer coating material for coating hydrophobic powder layer by layer as described in claim 1, It is characterized by: being stirring 0.5 hour in step A and step B, make to be uniformly mixed, 80 DEG C after the reaction was completed, filters.
3. such as the organosilane polymer coating material for coating hydrophobic powder layer by layer of any one of claim 1-2 the method preparation For preparing application of the special wetability coating in waterproofing agent.
4. a kind of as claimed in claim 3 using the organosilane polymer coating material prepares coating for coating hydrophobic powder layer by layer Method, it is characterised in that: by layer by layer coat hydrophobic powder organosilane polymer be scattered in toluene be uniformly mixed, pass through spray The mode of painting or dip-coating is coated with the waterproof coating of constructing super-drainage on base material.
5. the side as claimed in claim 4 using the organosilane polymer coating material prepares coating for coating hydrophobic powder layer by layer Method, it is characterised in that: take 40 mg to be scattered in 10 mL toluene the organosilane polymer for coating hydrophobic powder layer by layer, concussion makes to gather It is evenly dispersed to close object, is coated on base material sponge surface using dip coating, obtains the polymer coating with fire resistance characteristic.
CN201810449982.0A 2018-05-11 2018-05-11 A kind of preparation method and applications for the organosilane polymer coating material coating hydrophobic powder layer by layer Expired - Fee Related CN108893051B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104789124A (en) * 2014-12-30 2015-07-22 中国科学院兰州化学物理研究所 A preparing method of a stable superamphiphobic surface
CN105440888A (en) * 2015-12-17 2016-03-30 中国科学院兰州化学物理研究所 Preparation method of stable superhydrophobic hot liquid coating

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104789124A (en) * 2014-12-30 2015-07-22 中国科学院兰州化学物理研究所 A preparing method of a stable superamphiphobic surface
CN105440888A (en) * 2015-12-17 2016-03-30 中国科学院兰州化学物理研究所 Preparation method of stable superhydrophobic hot liquid coating

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