CN105622878A - Preparation method of waterborne waterproof coating - Google Patents
Preparation method of waterborne waterproof coating Download PDFInfo
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- CN105622878A CN105622878A CN201610109625.0A CN201610109625A CN105622878A CN 105622878 A CN105622878 A CN 105622878A CN 201610109625 A CN201610109625 A CN 201610109625A CN 105622878 A CN105622878 A CN 105622878A
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6685—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/83—Chemically modified polymers
- C08G18/837—Chemically modified polymers by silicon containing compounds
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/19—Quaternary ammonium compounds
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
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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
- 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
- C09D7/63—Additives non-macromolecular organic
Abstract
The invention discloses a preparation method of a waterborne waterproof coating. Polyether glycol and diisocyanate react to obtain an isocyanate-terminated polyurethane prepolymer; epoxy silane is dropwise added into the prepolymer, and reaction is kept at the temperature of 75-85 DEG C for 0.5-1.5 hours; cooling is performed to reach the temperature of 60-70 DEG C, a hydrophilic chain extender is dropwise added, and reaction is performed for 0.5-1.5 hours; cooling is performed to reach the temperature of 25-35 DEG C, a salt-forming agent is dropwise added, and reaction is performed for 20-30 minutes; distilled water and a chain extender are added, reaction is performed under strong stirring for 30-50 minutes; ammonium fluorocarboxylate is added, and strong stirring and even mixing are performed to obtain the epoxy silane/ammonium fluorocarboxylate/waterborne waterproof polyurethane coating. When the waterborne waterproof coating is used as a building wall material or an automobile surface coating or used for other applications, the waterproof performance is greatly improved compared with common waterborne polyurethane, and the application range of the waterborne polyurethane in the field of high-performance coatings is widened.
Description
Technical field
The invention belongs to technical field of coatings, it is specifically related to the preparation method of a kind of modified polyurethane aqueous waterproofing paint.
Background technology
The synthesis of aqueous polyurethane needs to introduce hydrophilic radical, thus causes surface tension excessive, and waterproof water tolerance is poor. Due to the restriction of synthesis technique, for solvent borne polyurethane material, the relative molecular mass of aqueous polyurethane dispersion is lower. In addition, self-emulsifying systems introduces hydrophilic radical again on its segment, such as amino (-NH2), hydroxyl (-COOH) or sulfonic group (-SO3Etc., H) these hydrophilic radicals make the water-repellancy of film be affected, it may also be useful in process, water tolerance is poor, it is easy to whiting and bubbling, limit the application of aqueous polyurethane coating in high-performance coating field.
The water-repellancy improving aqueous polyurethane has been done a lot of improvement by current researchist, and method of modifying is mainly divided into two classes, cross-linking modified and surface modification. Cross-linking modified being connected together by linear polyester macromolecular chain with the form of chemical bond, modified urethane has good water resistance; Surface modification reduces its surface tension by introducing low-surface-energy material in aqueous polyurethane emulsion, thus reaches the object improving water tolerance. But current most of system is all adopt single method or material that aqueous polyurethane is carried out modification, has certain limitation, can not improve its water tolerance most effectively.
Summary of the invention
The object of the invention is to provide a kind of epoxy radicals silicone hydride/carboxylic acid fluoride ammonium salt/polyurethane aqueous waterproof paint with excellent water resistance.
A preparation method for aqueous waterproofing paint, comprises the following steps:
1) isocyanate terminated base polyurethane prepolymer for use as is obtained by polyether Glycols and di-isocyanate reaction;
2) in performed polymer drip add epoxy radicals silicone hydride, at 75-85 DEG C keep reaction 0.5-1.5h;
3) it is cooled to 60-70 DEG C and adds hydrophilic chain extender, reaction 0.5-1.5h;
4) it is cooled to 25-35 DEG C, drips additive salt agent, reaction 20-30min;
5) add distilled water and chainextender, under strong stirring, react 30-50min;
6) adding carboxylic acid fluoride ammonium salt, strong stirring mixes, and obtains epoxy radicals silicone hydride/carboxylic acid fluoride ammonium salt/polyurethane aqueous waterproof paint;
Wherein, raw materials used meter by weight is as follows:
Polyether Glycols 15-25 part
Vulcabond 4-6.5 part
Epoxy radicals silicone hydride 1-1.5 part
Hydrophilic chain extender 1-1.5 part
Salt forming agent 0.8-1.1 part
Distilled water 50-70 part
Chainextender 0.2-0.4 part
Carboxylic acid fluoride ammonium salt 0.2-0.4 part.
By such scheme, described carboxylic acid fluoride ammonium salt is prepared by the following method:
With N-ethyl, N-hydroxyethyl perfluorinated octyl sulfuryl amine (DF-10) and Succinic anhydried are starting material, and DMF is solvent, and 4-bis-first nitrogen yl pyridines (DMAP) goes out carboxylic acid fluoride (FCA) for catalyst preparing; Taking carboxylic acid fluoride and TEA as starting material, synthesis is dissolved in the carboxylic acid fluoride salts solution of water.
By such scheme, step 1) mol ratio of isocyanate group and hydroxyl is 3:1.
By such scheme, described vulcabond is tolylene diisocyanate, diphenylmethanediisocyanate or hexamethylene diisocyanate.
By such scheme, described polyether Glycols to be molecular-weight average be 2000 polyoxyethylene glycol (PEG2000) or polypropylene glycol (PPG2000).
By such scheme, described hydrophilic chain extender is the two hydroxymethyl propionic acid (DMPA) of 2-2; Reaction system is added after being dissolved in N-N dimethyl formamide (DMF).
By such scheme, described epoxy radicals silicone hydride is ��-(2,3-ring oxygen third oxygen) propyl trimethoxy silicane (KH-560).
By such scheme, described salt forming agent is triethylamine (TEA).
By such scheme, described chainextender is quadrol (EDA).
For the problem that Water-resistance of Waterborne Polyurethane is poor; Adopt organosilicon and organic fluorine that it is carried out modification simultaneously. Epoxy radicals silicone hydride has lower surface tension, and epoxy group(ing) can be reacted with isocyano and be formed network structure simultaneously, stops moisture to enter coat inside; Carboxylic acid fluoride ammonium salt contains the functional group identical with aqueous polyurethane chain, and its aqueous solution can be blended with aqueous polyurethane emulsion, reduces the surface tension of emulsion, and carboxylic acid fluoride ammonium salt migrates to coatingsurface in coating film process.
Relative to prior art, the useful effect of the present invention is as follows:
Organic fluorine involved in the present invention is carboxylic acid fluoride ammonium salt, carboxylic acid fluoride ammonium salt aqueous solution and aqueous polyurethane contain identical functional group, there is good consistency, different from the past by grafting or copolymerization introducing organic fluorine, the organic fluorine molecule introduced by this method is less, film process more easily migrates to film coated surface, it is only necessary to add a small amount of organic fluorine and just can reach surface hydrophobicity effect.
The aqueous polyurethane coating of the present invention's synthesis has excellent water tolerance, and surface tension reduces greatly, and surface contact angle also reaches hydrophobic requirement.
When being used as other purposes such as construction material and car surface coating, comparing common water borne urethane, its water resistance obtains very big improvement, will expand the application of aqueous polyurethane in high-performance coating field.
Embodiment
Following examples explain the technical scheme of the present invention further, but not as limiting the scope of the invention.
The preparation process of carboxylic acid fluoride ammonium salt is as follows:
1) 55-65 DEG C, N-ethyl, N-hydroxyethyl perfluorinated octyl sulfuryl amine and Succinic anhydried are dissolved in N-N dimethyl formamide respectively;
2) N-ethyl, N-hydroxyethyl perfluorinated octyl sulfuryl amine solution and Succinic anhydried solution blending, 55-65 DEG C of insulation 25-35min;
3) it is warming up to 85-95 DEG C, adds catalyzer 4-bis-first nitrogen yl pyridines, reaction 7.5-8.5h;
4) pouring distilled water extraction fast into, filtering and washing rear drying for several times obtains carboxylic acid fluoride;
5) adding triethylamine aqueous solution in carboxylic acid fluoride, 20-30 DEG C of reaction 3-4h obtains carboxylic acid fluoride ammonium salt (FAC) solution.
Embodiment 1
PPG2000 is placed in there-necked flask, heats up and vacuumizes, and carries out processed, is 110 DEG C in interior temperature, and when vacuum tightness is 133.3Pa, the treatment time is 2.0h; Adding PPG2000 in reactor, drip wherein and add TDI, the lower 75 DEG C of reaction 0.5h of nitrogen atmosphere, add catalyzer, and 80 DEG C of reaction 1.0h obtain base polyurethane prepolymer for use as, and in reaction process, rotating speed remains on 60r/min.
Maintenance system 80 DEG C, drip add KH-560, rate of addition be two seconds one, stirring reaction 1.0h, rotating speed 60r/min; Be cooled to 65 DEG C, drip add DMPA, rate of addition be two seconds one, stirring reaction 1.0h, rotating speed 60r/min; Be cooled to 30 DEG C, drip add TEA, rate of addition be two seconds one, reaction 20min, rotating speed 120r/min; Add distilled water and EDA, under strong stirring, react 40min; Receive sample after having reacted and obtain epoxy radicals silicone hydride modified aqueous polyurethane emulsion.
Accurately take FAC solution, join epoxy radicals silicone hydride modified aqueous polyurethane emulsion, strong stirring 30min, rotating speed 180r/min. Receive sample after having reacted and obtain epoxy radicals silicone hydride/carboxylic acid fluoride ammonium salt/polyurethane aqueous waterproof paint.
Test the correlated performance of epoxy radicals silicone hydride/carboxylic acid fluoride ammonium salt/polyurethane aqueous waterproof paint by associated test standards, the surface tension of coating is 17.9mN/m; After film soaks 24h in water, water-intake rate is 7.14%; Surface hydrophobicity angle is 114 ��.
Embodiment 2
PPG2000 is placed in there-necked flask, heats up and vacuumizes, and carries out processed, is 110 DEG C in interior temperature, and when vacuum tightness is 133.3Pa, the treatment time is 2.0h; Adding PPG2000 in reactor, drip wherein and add MDI, the lower 75 DEG C of reaction 0.5h of nitrogen atmosphere, add catalyzer, and 80 DEG C of reaction 1.0h, in reaction process, rotating speed remains on 60r/min.
Maintenance system 82 DEG C, drip add KH-560, rate of addition be two seconds one, stirring reaction 0.7h, rotating speed 60r/min; Be cooled to 68 DEG C, drip add DMPA, rate of addition be two seconds one, stirring reaction 0.7h, rotating speed 60r/min; Be cooled to 32 DEG C, drip add TEA, rate of addition be two seconds one, reaction 22min, rotating speed 120r/min; Add distilled water and EDA, under strong stirring, react 45min; Receive sample after having reacted and obtain epoxy radicals silicone hydride modified aqueous polyurethane emulsion.
Accurately take FAC solution, join epoxy radicals silicone hydride modified aqueous polyurethane emulsion, strong stirring 30min, rotating speed 180r/min. Receive sample after having reacted and obtain epoxy radicals silicone hydride/carboxylic acid fluoride ammonium salt/polyurethane aqueous waterproof paint.
Test the correlated performance of epoxy radicals silicone hydride/carboxylic acid fluoride ammonium salt/polyurethane aqueous waterproof paint by associated test standards, the surface tension of coating is 18.0mN/m; After film soaks 24h in water, water-intake rate is 7.26%; Surface hydrophobicity angle is 113 ��.
Embodiment 3
PPG2000 is placed in there-necked flask, heats up and vacuumizes, and carries out processed, is 110 DEG C in interior temperature, and when vacuum tightness is 133.3Pa, the treatment time is 2.0h; Adding PPG2000 in reactor, drip wherein and add HDI, the lower 75 DEG C of reaction 0.5h of nitrogen atmosphere, add catalyzer, and 80 DEG C of reaction 1.0h, in reaction process, rotating speed remains on 60r/min.
Maintenance system 80 DEG C, drip add KH-560, rate of addition be two seconds one, stirring reaction 1.2h, rotating speed 60r/min; Be cooled to 65 DEG C, drip add DMPA, rate of addition be two seconds one, stirring reaction 1.2h, rotating speed 60r/min; Be cooled to 30 DEG C, drip add TEA, rate of addition be two seconds one, reaction 30min, rotating speed 120r/min; Add distilled water and EDA, under strong stirring, react 40min; Receive sample after having reacted and obtain epoxy radicals silicone hydride modified aqueous polyurethane emulsion.
Accurately take FAC solution, join epoxy radicals silicone hydride modified aqueous polyurethane emulsion, strong stirring 30min, rotating speed 180r/min. Receive sample after having reacted and obtain epoxy radicals silicone hydride/carboxylic acid fluoride ammonium salt/polyurethane aqueous waterproof paint.
Test the correlated performance of epoxy radicals silicone hydride/carboxylic acid fluoride ammonium salt/polyurethane aqueous waterproof paint by associated test standards, the surface tension of coating is 18.1mN/m; After film soaks 24h in water, water-intake rate is 7.35%; Surface hydrophobicity angle is 110 ��.
Embodiment 4
PEG2000 is placed in there-necked flask, heats up and vacuumizes, and carries out processed, is 110 DEG C in interior temperature, and when vacuum tightness is 133.3Pa, the treatment time is 2.0h; Adding PPG2000 in reactor, drip wherein and add TDI, the lower 75 DEG C of reaction 0.5h of nitrogen atmosphere, add catalyzer, and 80 DEG C of reaction 1.0h, in reaction process, rotating speed remains on 60r/min.
Maintenance system 78 DEG C, drip add KH-560, rate of addition be two seconds one, stirring reaction 1.2h, rotating speed 60r/min; Be cooled to 70 DEG C, drip add DMPA, rate of addition be two seconds one, stirring reaction 1.0h, rotating speed 60r/min; Be cooled to 28 DEG C, drip add TEA, rate of addition be two seconds one, reaction 35min, rotating speed 120r/min; Add distilled water and EDA, under strong stirring, react 45min; Receive sample after having reacted and obtain epoxy radicals silicone hydride modified aqueous polyurethane emulsion.
Accurately take FAC solution, join epoxy radicals silicone hydride modified aqueous polyurethane emulsion, strong stirring 30min, rotating speed 180r/min. Receive sample after having reacted and obtain epoxy radicals silicone hydride/carboxylic acid fluoride ammonium salt/polyurethane aqueous waterproof paint.
Test the correlated performance of epoxy radicals silicone hydride/carboxylic acid fluoride ammonium salt/polyurethane aqueous waterproof paint by associated test standards, the surface tension of coating is 18.1mN/m; After film soaks 24h in water, water-intake rate is 7.32%; Surface hydrophobicity angle is 112 ��.
Embodiment 5
PEG2000 is placed in there-necked flask, heats up and vacuumizes, and carries out processed, is 110 DEG C in interior temperature, and when vacuum tightness is 133.3Pa, the treatment time is 2.0h; Adding PPG2000 in reactor, drip wherein and add MDI, the lower 75 DEG C of reaction 0.5h of nitrogen atmosphere, add catalyzer, and 80 DEG C of reaction 1.0h, in reaction process, rotating speed remains on 60r/min.
Maintenance system 85 DEG C, drip add KH-560, rate of addition be two seconds one, stirring reaction 0.7h, rotating speed 60r/min; Be cooled to 70 DEG C, drip add DMPA, rate of addition be two seconds one, stirring reaction 0.7h, rotating speed 60r/min; Be cooled to 25 DEG C, drip add TEA, rate of addition be two seconds one, reaction 30min, rotating speed 120r/min; Add distilled water and EDA, under strong stirring, react 40min; Receive sample after having reacted and obtain epoxy radicals silicone hydride modified aqueous polyurethane emulsion.
Accurately take FAC solution, join epoxy radicals silicone hydride modified aqueous polyurethane emulsion, strong stirring 30min, rotating speed 180r/min. Receive sample after having reacted and obtain epoxy radicals silicone hydride/carboxylic acid fluoride ammonium salt/polyurethane aqueous waterproof paint.
Test the correlated performance of epoxy radicals silicone hydride/carboxylic acid fluoride ammonium salt/polyurethane aqueous waterproof paint by associated test standards, the surface tension of coating is 17.9mN/m; After film soaks 24h in water, water-intake rate is 7.19%; Surface hydrophobicity angle is 114 ��.
Claims (9)
1. the preparation method of an aqueous waterproofing paint, it is characterised in that comprise the following steps:
1) isocyanate terminated base polyurethane prepolymer for use as is obtained by polyether Glycols and di-isocyanate reaction;
2) in performed polymer drip add epoxy radicals silicone hydride, at 75-85 DEG C keep reaction 0.5-1.5h;
3) it is cooled to 60-70 DEG C and adds hydrophilic chain extender, reaction 0.5-1.5h;
4) it is cooled to 25-35 DEG C, drips additive salt agent, reaction 20-30min;
5) add distilled water and chainextender, under strong stirring, react 30-50min;
6) adding carboxylic acid fluoride ammonium salt, strong stirring mixes, and obtains epoxy radicals silicone hydride/carboxylic acid fluoride ammonium salt/polyurethane aqueous waterproof paint;
Wherein, raw materials used meter by weight is as follows:
Polyether Glycols 15-25 part
Vulcabond 4-6.5 part
Epoxy radicals silicone hydride 1-1.5 part
Hydrophilic chain extender 1-1.5 part
Salt forming agent 0.8-1.1 part
Distilled water 50-70 part
Chainextender 0.2-0.4 part
Carboxylic acid fluoride ammonium salt 0.2-0.4 part.
2. the preparation method of aqueous waterproofing paint as claimed in claim 1, it is characterised in that described carboxylic acid fluoride ammonium salt is prepared by the following method:
With N-ethyl, N-hydroxyethyl perfluorinated octyl sulfuryl amine (DF-10) and Succinic anhydried are starting material, and DMF is solvent, and 4-bis-first nitrogen yl pyridines (DMAP) goes out carboxylic acid fluoride (FCA) for catalyst preparing; Taking carboxylic acid fluoride and TEA as starting material, synthesis is dissolved in the carboxylic acid fluoride salts solution of water.
3. the preparation method of aqueous waterproofing paint as claimed in claim 1, it is characterised in that step 1) mol ratio of isocyanate group and hydroxyl is 3:1.
4. the preparation method of aqueous waterproofing paint as claimed in claim 1, it is characterised in that described vulcabond is tolylene diisocyanate, diphenylmethanediisocyanate or hexamethylene diisocyanate.
5. the preparation method of aqueous waterproofing paint as claimed in claim 1, it is characterised in that described polyether Glycols to be molecular-weight average be 2000 polyoxyethylene glycol or polypropylene glycol.
6. the preparation method of aqueous waterproofing paint as claimed in claim 1, it is characterised in that described hydrophilic chain extender is the two hydroxymethyl propionic acid of 2-2; Reaction system is added after being dissolved in N-N dimethyl formamide.
7. the preparation method of aqueous waterproofing paint as claimed in claim 1, it is characterised in that described epoxy radicals silicone hydride is ��-(2,3-ring oxygen third oxygen) propyl trimethoxy silicane.
8. the preparation method of aqueous waterproofing paint as claimed in claim 1, it is characterised in that described salt forming agent is triethylamine.
9. the preparation method of aqueous waterproofing paint as claimed in claim 1, it is characterised in that described chainextender is quadrol.
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Cited By (5)
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| CN106497385A (en) * | 2016-11-23 | 2017-03-15 | 四川大学 | A kind of preparation method of visible ray selfreparing aqueous polyurethane coating material of the main chain containing double selenium keys |
| CN107200849A (en) * | 2017-05-17 | 2017-09-26 | 江苏超力建材科技有限公司 | A kind of cement road seam aqueous interfacial agents and its preparation method and application |
| CN112077964A (en) * | 2020-09-21 | 2020-12-15 | 柳州唐辰木业有限公司 | Waterproof stain-resistant wood packaging box material and preparation method thereof |
| CN113502114A (en) * | 2021-07-07 | 2021-10-15 | 上海库曜新材料有限公司 | Two-component ultra-fast-drying weather-resistant hydrophobic and oleophobic polyurea finish paint |
| CN113957719A (en) * | 2021-11-12 | 2022-01-21 | 南通大学 | Organic silicon polyurethane waterproof moisture permeable coating agent and preparation method and finishing process thereof |
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| CN1854165A (en) * | 2005-04-20 | 2006-11-01 | 广州宏昌胶粘带厂 | Organic silicon modified aqueous polyurethane |
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| CN107200849B (en) * | 2017-05-17 | 2020-06-09 | 江苏超力建材科技有限公司 | Water-based interface agent for cement highway joint and preparation method and application thereof |
| CN112077964A (en) * | 2020-09-21 | 2020-12-15 | 柳州唐辰木业有限公司 | Waterproof stain-resistant wood packaging box material and preparation method thereof |
| CN113502114A (en) * | 2021-07-07 | 2021-10-15 | 上海库曜新材料有限公司 | Two-component ultra-fast-drying weather-resistant hydrophobic and oleophobic polyurea finish paint |
| CN113957719A (en) * | 2021-11-12 | 2022-01-21 | 南通大学 | Organic silicon polyurethane waterproof moisture permeable coating agent and preparation method and finishing process thereof |
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