CN107987657A - A kind of preparation method of water-repellent paint - Google Patents
A kind of preparation method of water-repellent paint Download PDFInfo
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- CN107987657A CN107987657A CN201711283489.8A CN201711283489A CN107987657A CN 107987657 A CN107987657 A CN 107987657A CN 201711283489 A CN201711283489 A CN 201711283489A CN 107987657 A CN107987657 A CN 107987657A
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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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
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- Health & Medical Sciences (AREA)
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Abstract
A kind of preparation method of water-repellent paint, it is characterised in that this method comprises the following steps：The surface of nano-particle is modified, the preparation of hydrophobic resin and the preparation of coating, preparation method of the invention have the advantages that technique is simple and convenient, pollution-free, environmental-friendly, film quality is high, input-output ratio is high, of low cost and application prospect is extensive.
Description
Technical field
The present invention relates to a kind of preparation method of water-repellent paint.
Background technology
Waterproof material is that the building enclosure of building will prevent the infiltration of rainwater, snow-broth and underground water；Prevent in air
Moisture, steam and other pernicious gases and liquid erosion；Separation structure will prevent oozing for plumbing from turning over.These are impermeable,
Leakage and the material corroded are referred to as.Prevent in rainwater, underground water, industry and civilian plumbing, corrosive liquids and air
Moisture, the material of the intrusion building such as steam.Building need carry out water-proofing treatment position be mainly roofing, metope,
Face and basement.
The waterproof material of in the market has two major classes：First, polyurethanes water-repellent paint.This kind of material is usually by polyurethane
It is made with coal tar as raw material.The tar gas toxicity that it is volatilized is big, and does not allow easy-clear, therefore in 2000 in China
It is prohibited from using.It is to be used as raw material instead of coal tar by the use of pitch still in the polyurethane waterproofing coating of sale.But using this painting
It is general using being diluted containing organic solvents such as toluene, dimethylbenzene during material, thus also contain toxic；Another kind of is polymer water
Cement-base waterproof coating.It, with being formed mixed with the high grade cement of various additives, is polymerize by the lotion that a variety of waterborne polymerics synthesize
The flexibility of thing (resin) and the rigidity of cement became one so that it is excellent with being showed in terms of stability in impermeability.It excellent
Point is easy for construction, comprehensive cost low, short time limit, and asepsis environment-protecting.Therefore, polyalcohol cement basis has become water-repellent paint city
The leading role of field.
But current water-repellent paint also has the disadvantage that, such as poor performance, the characteristics of stability is not strong.
The content of the invention
The purpose of patent of the present invention is to provide a kind of preparation method of water-repellent paint, of the invention to use following technical side
Case：
A kind of preparation method of water-repellent paint, it is characterised in that this method comprises the following steps：
Step 1, the nano-particle that surface is modified
Nano-silicon dioxide particle and deionized water are mixed and carry out ultrasonic disperse 5-30min, adds ammonium hydroxide by mixed liquor
PH value adjust to 8-10, add dichloromethane and persistently stir 30-60min, reaction system is warming up to 40-60 after stirring
P-aminobenzene sulfonic acid DEG C is added, when keeping sonic oscillation reaction 1-5 small, ice bath is cooled to 0 DEG C, is added slowly with stirring Asia
Sodium nitrate aqueous solution, react 1h, be warming up to 40 DEG C, continue to stir lower reaction 1.5-2.5h, then mixed liquor is filtered with
Remove solvent, and be washed with deionized 3-6 time, finally by filtrate dry 24-48 it is small when obtain the nano-particle of sulfonation；
Step 2: the preparation of hydrophobic resin
Under nitrogen protection, by isoflurane chalcone diisocyanate or polyether acrylate, be warming up to 60-70 DEG C, add
The lower insulation 4-7h of Hexafluorobutyl mathacrylate stirring, 40-50 DEG C of cooling adds butyl acetate and azodiisobutyronitrile persistently stirs
Mix 2-5h and both obtain hydrophobic resin；
Step 3: the preparation of coating
Polystyrene emulsion, step 1 are prepared into the nano-particle of surface modification and step 2 prepares hydrophobic resin, acid
Acid anhydride is using mass ratio as 5-15:3-10:20-40:1-10, which is uniformly mixed, both obtains preventing water coating.
2nd, a kind of preparation method of water-repellent paint as claimed in claim 1, it is characterised in that nanometer described in step 1
Silicon dioxide granule, deionized water, dichloromethane, p-aminobenzene sulfonic acid, the mass ratio of sodium nitrite in aqueous solution is 5-10:50-
100:0.5-1:2-4:1-3。
3rd, a kind of preparation method of water-repellent paint as claimed in claim 2, it is characterised in that nanometer described in step 1
Silicon dioxide granule, deionized water, dichloromethane, p-aminobenzene sulfonic acid, the mass ratio of sodium nitrite in aqueous solution is 8:80:0.6:
3:2。
4th, a kind of preparation method of water-repellent paint as claimed in claim 1, it is characterised in that nanometer described in step 1
The particle diameter of silicon dioxide granule is 2-10nm.
5th, a kind of preparation method of water-repellent paint as claimed in claim 1, it is characterised in that different fluorine described in step 2
Your ketone diisocyanate or polyether acrylate, Hexafluorobutyl mathacrylate, the matter of butyl acetate and azodiisobutyronitrile
It is 0.5-2 to measure ratio:3-7:5-10:0.1-0.8.
6th, a kind of preparation method of water-repellent paint as claimed in claim 5, it is characterised in that different fluorine described in step 2
Your ketone diisocyanate or polyether acrylate, Hexafluorobutyl mathacrylate, the matter of butyl acetate and azodiisobutyronitrile
Amount is than being 1:5:8:0.3.
Beneficial effect：
1st, preparation method of the invention is with technique is simple and convenient, pollution-free, environmental-friendly, film quality is high, input production
Go out the advantages that more extensive than high, of low cost and application prospect；
2nd, the coating intensity is big, and corrosion resistance is good.
Embodiment
With reference to specific embodiment, the present invention is further explained.
A kind of preparation method of water-repellent paint, it is characterised in that this method comprises the following steps：
Step 1, the nano-particle that surface is modified
Nano-silicon dioxide particle and deionized water are mixed and carry out ultrasonic disperse 5-30min, adds ammonium hydroxide by mixed liquor
PH value adjust to 8-10, add dichloromethane and persistently stir 30-60min, reaction system is warming up to 40-60 after stirring
P-aminobenzene sulfonic acid DEG C is added, when keeping sonic oscillation reaction 1-5 small, ice bath is cooled to 0 DEG C, is added slowly with stirring Asia
Sodium nitrate aqueous solution, react 1h, be warming up to 40 DEG C, continue to stir lower reaction 1.5-2.5h, then mixed liquor is filtered with
Remove solvent, and be washed with deionized 3-6 time, finally by filtrate dry 24-48 it is small when obtain the nano-particle of sulfonation；
Step 2: the preparation of hydrophobic resin
Under nitrogen protection, by isoflurane chalcone diisocyanate or polyether acrylate, be warming up to 60-70 DEG C, add
The lower insulation 4-7h of Hexafluorobutyl mathacrylate stirring, 40-50 DEG C of cooling adds butyl acetate and azodiisobutyronitrile persistently stirs
Mix 2-5h and both obtain hydrophobic resin；
Step 3: the preparation of coating
Polystyrene emulsion, step 1 are prepared into the nano-particle of surface modification and step 2 prepares hydrophobic resin, acid
Acid anhydride is using mass ratio as 5-15:3-10:20-40:1-10, which is uniformly mixed, both obtains preventing water coating.
Nano-silicon dioxide particle described in step 1, deionized water, dichloromethane, p-aminobenzene sulfonic acid, sodium nitrite
The mass ratio of aqueous solution is 5-10:50-100:0.5-1:2-4:1-3.
Nano-silicon dioxide particle described in step 1, deionized water, dichloromethane, p-aminobenzene sulfonic acid, sodium nitrite
The mass ratio of aqueous solution is 8:80:0.6:3:2.
The particle diameter of nano-silicon dioxide particle described in step 1 is 2-10nm.
Isoflurane chalcone diisocyanate described in step 2 or polyether acrylate, Hexafluorobutyl mathacrylate, second
The mass ratio of acid butyl ester and azodiisobutyronitrile is 0.5-2:3-7:5-10:0.1-0.8.
Isoflurane chalcone diisocyanate described in step 2 or polyether acrylate, Hexafluorobutyl mathacrylate, second
The mass ratio of acid butyl ester and azodiisobutyronitrile is 1:5:8:0.3.
(1) heretofore described polystyrene emulsion is prepared with the following method：
A, the preparation of styrene emulsion
Styrene and ammonium persulfate are placed in the container equipped with 40-55 DEG C of water, 20-60min is stirred, is passed through nitrogen, stirs
Azo-bis-isobutyrate hydrochloride and ammonium hydrogen carbonate are added while mixing, 40-55 DEG C of stirring 30-60min is kept, is warming up to 60~90
DEG C, reaction 3-15h is obtained, styrene emulsion；
The mass ratio of the styrene, ammonium persulfate, azo-bis-isobutyrate hydrochloride and ammonium hydrogen carbonate is 10-20:2-6:
1-3:3-7；
B, the preparation of cyclodextrine derivatives
(1) pretreatment of beta-cyclodextrin：
Distilled water is added in a reservoir, is heated to 90-100 DEG C, takes beta-cyclodextrin to be placed in heated steaming under agitation
Dissolved in distilled water, keep temperature control to be filtered at 90-95 DEG C, 10-20h at a temperature of filtrate is placed in -5-5 DEG C so that
Crystal separates out, and the crystal of precipitation, which is placed on, to dry when 6 is small in 80 DEG C of vacuum drying chambers must crystallize beta-cyclodextrin；The distillation
The mass ratio of water and beta-cyclodextrin is 100-200:20-30；
(2) preparation of cyclodextrine derivatives
Beta-cyclodextrin of the step (1) by pretreatment is placed in anhydrous pyridine, 15- is stirred in -5-0 DEG C of ice-water bath
Mixed liquor is made in 60min, NaOH and deionized water is added in mixed liquor the liquid that pH value is 9-11 is made, be warming up to 25-30
Butyrolactone DEG C is added in the liquid, reacts 15-30min, is cooled to -5-0 DEG C again, 1,2- epoxy butanes is added and keeps temperature
3-6h is reacted, adds second eyeball solution sustained response 10-15h, after completion of the reaction, pH value is adjusted to neutrality using hydrochloric acid, is used
Vacuum rotary steam removes water and pyridine, and solid particle is placed in dimethylformamide and is stirred evenly, is consolidated using acetone precipitation
Body product, is dried in vacuo 3-6h at 70-90 DEG C by the product and obtains solid particle, is cyclodextrine derivatives；
The beta-cyclodextrin of the pretreatment, anhydrous pyridine, butyrolactone, 1,2- epoxy butane, the mass ratio of second eyeball is 10-
20:30-60:2-5:3-6:1-3；
C, the preparation of polystyrene emulsion
Cyclodextrine derivatives and deionized water prepared by styrene emulsion, step B prepared by step A are mixed equal
It is even, n-butanol and n,N-dimethylacetamide are added, is passed through nitrogen temperature to 50 DEG C, when reaction 3-6 is small, stops heating and stirring
Mix down and be cooled to room temperature, obtain polystyrene emulsion；
The mass ratio of the styrene emulsion, cyclodextrine derivatives, deionized water, n-butanol and n,N-dimethylacetamide
For 5-10:1-3:30-60:2-4:3-5；
(2) research is found
1st, cyclodextrine derivatives prepared in the present invention are 2-O- (2- hydroxybutyls)-cyclodextrin, and yield can reach
12-16%, far more than the yield of 6-9% on the market, this is because the beta-cyclodextrin of pretreatment is placed in nothing first in the present invention
In water pyridine, mixed at a temperature of -5-0 DEG C of ice-water bath, by adding butyrolactone after heating, be cooled to -5-0 DEG C of ice again
1,2- epoxy butanes under water-bath, research are found, are added different materials by the change of this temperature, can effectively be lifted pre- place
The reactivity of the beta-cyclodextrin of reason, so as to lift the yield of cyclodextrine derivatives by about one time；
2nd, in addition research is found, is spread out using the beta-cyclodextrin of pretreatment compared to direct using beta-cyclodextrin production cyclodextrin
Biology, its yield can lift 1-2%；
3rd, find by research, lifted by adding cyclodextrine derivatives polystyrene emulsion shelf stability, with
Do not add cyclodextrin as a comparison embodiment 1, add beta-cyclodextrin embodiment 2 as a comparison, adding cyclodextrin with the present invention spreads out
Biology is compared, referring specifically to table 1.Table 1
| Comparative example 1 | Comparative example 2 | Add cyclodextrine derivatives | |
| Storage 1 week | Lotion is substantially layered | It is unchanged | It is unchanged |
| Storage 1 month | Creaming of emulsion, flocculation are serious | It is unchanged | It is unchanged |
| Store 2-3 months | Creaming of emulsion, flocculation are serious | Without obvious layering | It is unchanged |
| Store 4-6 months | Creaming of emulsion, flocculation are serious | Creaming of emulsion, flocculation are serious | It is unchanged |
4th, found by studying, the reaction time of polystyrene emulsion can effectively be lifted by adding cyclodextrine derivatives；With benzene
The mass ratio of vac emulsion, cyclodextrine derivatives, deionized water, n-butanol and n,N-dimethylacetamide is 6:1.5:50:3:
The conversion ratio that styrene is tested exemplified by 3.5 is shown in Table 2.
Table 2
| Comparative example 1 | Comparative example 2 | Add cyclodextrine derivatives | |
| React 3h | 30% | 76% | 92% |
| React 5h | 65% | Less than 95% | More than 98% |
| React 6h | 65% | Less than 95% | More than 98% |
5th, surface modification is carried out for nano-silicon dioxide particle in the present invention, is handled using sulfonating surface, rather than it is existing
There is common surface hydroxyl processing in technology, found by studying, its surface and institute in the present invention after being handled using sulfonating surface
Bond conjunction between the polystyrene emulsion and hydrophobic resin stated is even closer, can effectively strengthen coating property, referring specifically to
Table 3.
Table 3
It is to be understood that these embodiments are only illustrative of the invention and is not intended to limit the scope of the invention.In addition, it should also be understood that,
After reading the content taught by the present invention, those skilled in the art can make various modifications or changes to the present invention, these
Equivalent form is also fallen within the scope of the appended claims of the present application.
Claims (6)
1. a kind of preparation method of water-repellent paint, it is characterised in that this method comprises the following steps：
Step 1, the nano-particle that surface is modified
Nano-silicon dioxide particle and deionized water are mixed and carry out ultrasonic disperse 5-30min, adds ammonium hydroxide by the pH of mixed liquor
Value is adjusted to 8-10, is added dichloromethane and is persistently stirred 30-60min, reaction system is warming up to 40-60 DEG C again after stirring
P-aminobenzene sulfonic acid is added, when keeping sonic oscillation reaction 1-5 small, ice bath is cooled to 0 DEG C, is added slowly with stirring nitrous acid
Sodium water solution, reacts 1h, is warming up to 40 DEG C, continues to stir lower reaction 1.5-2.5h, then mixed liquor is filtered to remove
Solvent, and being washed with deionized 3-6 times, finally by filtrate drying 24-48 it is small when obtain the nano-particle of sulfonation；
Step 2: the preparation of hydrophobic resin
Under nitrogen protection, by isoflurane chalcone diisocyanate or polyether acrylate, be warming up to 60-70 DEG C, add methyl
The lower insulation 4-7h of hexafluorobutyl acrylate stirring, is cooled to 40-50 DEG C of addition butyl acetate and azodiisobutyronitrile persistently stirs
2-5h both obtains hydrophobic resin；
Step 3: the preparation of coating
By polystyrene emulsion, step 1 prepare surface be modified nano-particle, step 2 prepare hydrophobic resin and acid anhydrides with
Mass ratio is 5-15:3-10:20-40:1-10, which is uniformly mixed, both obtains preventing water coating.
A kind of 2. preparation method of water-repellent paint as claimed in claim 1, it is characterised in that nano-silica described in step 1
SiClx particle, deionized water, dichloromethane, p-aminobenzene sulfonic acid, the mass ratio of sodium nitrite in aqueous solution is 5-10:50-100:
0.5-1:2-4:1-3。
A kind of 3. preparation method of water-repellent paint as claimed in claim 2, it is characterised in that nano-silica described in step 1
SiClx particle, deionized water, dichloromethane, p-aminobenzene sulfonic acid, the mass ratio of sodium nitrite in aqueous solution is 8:80:0.6:3:2.
A kind of 4. preparation method of water-repellent paint as claimed in claim 1, it is characterised in that nano-silica described in step 1
The particle diameter of SiClx particle is 2-10nm.
A kind of 5. preparation method of water-repellent paint as claimed in claim 1, it is characterised in that isophorone described in step 2
Diisocyanate or polyether acrylate, Hexafluorobutyl mathacrylate, the mass ratio of butyl acetate and azodiisobutyronitrile
For 0.5-2:3-7:5-10:0.1-0.8.
A kind of 6. preparation method of water-repellent paint as claimed in claim 5, it is characterised in that isophorone described in step 2
Diisocyanate or polyether acrylate, Hexafluorobutyl mathacrylate, the mass ratio of butyl acetate and azodiisobutyronitrile
For 1:5:8:0.3.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108084865A (en) * | 2017-12-15 | 2018-05-29 | 安徽省华腾农业科技有限公司 | A kind of preparation method of water-repellent paint |
| CN108676451A (en) * | 2018-05-21 | 2018-10-19 | 张家港宝视特影视器材有限公司 | Diffusing reflection coating material, high-resolution white plastic curtain cloth and preparation method thereof |
| CN109354985A (en) * | 2018-09-05 | 2019-02-19 | 江苏叙然信息科技有限公司 | A kind of high security waterproof material |
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| CN108084865A (en) * | 2017-12-15 | 2018-05-29 | 安徽省华腾农业科技有限公司 | A kind of preparation method of water-repellent paint |
| CN108676451A (en) * | 2018-05-21 | 2018-10-19 | 张家港宝视特影视器材有限公司 | Diffusing reflection coating material, high-resolution white plastic curtain cloth and preparation method thereof |
| CN109354985A (en) * | 2018-09-05 | 2019-02-19 | 江苏叙然信息科技有限公司 | A kind of high security waterproof material |
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