CN106811066A - The preparation method of aqueous polyurethane coating - Google Patents
The preparation method of aqueous polyurethane coating Download PDFInfo
- Publication number
- CN106811066A CN106811066A CN201510865728.5A CN201510865728A CN106811066A CN 106811066 A CN106811066 A CN 106811066A CN 201510865728 A CN201510865728 A CN 201510865728A CN 106811066 A CN106811066 A CN 106811066A
- Authority
- CN
- China
- Prior art keywords
- aqueous polyurethane
- coating
- added
- reactor
- polyurethane coating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Polyurethanes Or Polyureas (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses the preparation method of aqueous polyurethane coating, including following operation：1）At room temperature to IPDI etc. is added in the first reactor, primary product is obtained；2）To dihydromethyl propionic acid is added in primary product, triethylamine is added, Aliphatic Polyester Aqueous Polyurethane Dispersions are obtained；3）Modified silicasol is obtained；4）At room temperature to Aliphatic Polyester Aqueous Polyurethane Dispersions and modified silicasol is added in the 3rd reactor, mixed emulsion is obtained；5）To appropriate acrylic acid copolymer sodium salt etc. is added in the 4th reactor for filling distilled water, obtain mixing bottom liquid；6）To mixed emulsion is added in mixing bottom liquid, aqueous polyurethane coating is obtained.Effective closing can be carried out to protected object using coating obtained in the present invention to protect, and prevented protected object to be contaminated, corrode and damaged.Meanwhile, the coating also has the advantages that strippable property is good, coating strength is high, cohesive force is strong and stability is high.
Description
Technical field
The present invention relates to decorating field, more particularly, to the preparation method of aqueous polyurethane coating.
Background technology
To prevent material or half product under the atmospheric environment to be contaminated, corrode and damage, and increase the service life, it will usually there is the coating of good protective and strippable property in their surface smear it is carried out effective and interim to seal protection up for safekeeping.In this way, can both isolate air, salt fog, the invasion of microorganism in the external world, antiseptic effect is reached；The effect of decontamination can be cleaned to reach by adsorbing pollutant again.For compared with solvent-borne type protective coating, aqueous protective coating has more security and the feature of environmental protection, thus is widely used in the decorating field of product.But, existing aqueous protective coating still has the shortcomings that coating strength is low, strippable property is poor and barrier propterty is single.
The content of the invention
The purpose of the present invention is the defect for overcoming above-mentioned prior art; the preparation method of aqueous polyurethane coating is provided; effective closing can be carried out to protected object using coating obtained in the present invention to protect, and have the advantages that strippable property is good, coating strength is high, cohesive force is strong and stability is high.
The purpose of the present invention is achieved through the following technical solutions：
The preparation method of aqueous polyurethane coating, including following operation：
1）At room temperature to addition IPDI, polypropylene glycol, polyethylene glycol, dibutyl tin laurate and butanone in the first reactor, temperature is risen to 58 ~ 80 DEG C again, their-NCO% values in hybrid reaction to system in the first reactor is no longer changed, obtain primary product, it is standby；
2）By temperature control at 80 DEG C, to operation 1）Dihydromethyl propionic acid is added in the primary product of gained and 220 ~ 260min is reacted, then cools the temperature to 38 ~ 43 DEG C, addition triethylamine obtains secondary product；To adding secondary product in the second reactor for filling distilled water and secondary product is scattered in distilled water, the diethylenetriamine aqueous solution is added, Aliphatic Polyester Aqueous Polyurethane Dispersions are obtained；
3）To propyl trimethoxy silicane is added in the flask for filling ethanol, by the rotating speed stirring 5 ~ 10min of mixing of 100 ~ 200r/min, solution of silane is obtained；Rotating speed is controlled for 200 ~ 300r/min, to solution of silane is added dropwise in the 3rd reactor for filling alkaline silica sol；After completion of dropping, at a temperature of 50 ~ 65 DEG C, by the rotating speed stirring 450 ~ 500min of mixing of 250r/min, modified silicasol is obtained, it is standby；
4）At room temperature to addition operation 2 in the 4th reactor）The Aliphatic Polyester Aqueous Polyurethane Dispersions and operation 3 of gained）The modified silicasol of gained, by the rotating speed stirring 50 ~ 70min of mixing of 200 ~ 300r/min, obtains mixed emulsion, standby；
5）To adding the swollen acrylic thickener of appropriate acrylic acid copolymer sodium salt, alkali soluble and organic silicon modified by polyether in the 5th reactor for filling distilled water, by the 4 ~ 10min of rotating speed stirring mixing of 200 ~ 300r/min, add appropriate titanium dioxide, mica, by the rotating speed stirring 35 ~ 42min of mixing of 1500 ~ 1800r/min, obtain mixing bottom liquid；
6）To operation 5）Operation 4 is added in the mixing bottom liquid of gained）The mixed emulsion of gained, by the 12 ~ 22min of rotating speed stirring mixing of 350 ~ 500r/min；Appropriate neopelex, polyether-modified dimethyl siloxane, alkali soluble is swollen acrylic thickener, aqueous silicone oil, organic silicon modified by polyether are added, by the rotating speed stirring 15 ~ 20min of mixing of 200 ~ 300r/min, aqueous polyurethane coating is obtained；
The modified silicasol is obtained by the raw material of following quality proportioning：40 ~ 60 parts of alkaline silica sol, 30 ~ 50 parts of ethanol, 1 ~ 6 part of propyl trimethoxy silicane；The Aliphatic Polyester Aqueous Polyurethane Dispersions are obtained by the raw material of following quality proportioning：40 ~ 80 parts of IPDI, 25 ~ 40 parts of polypropylene glycol, 25 ~ 80 parts of polyethylene glycol, 3 ~ 10 parts of dihydromethyl propionic acid, 50 ~ 80 parts of butanone, 5 ~ 12 parts of diethylenetriamine, 3 ~ 9 parts of triethylamine, 1 ~ 3 part of dibutyl tin laurate, 40 ~ 80 parts of distilled water；The aqueous polyurethane coating is obtained by the raw material of following mass fraction：Aliphatic Polyester Aqueous Polyurethane Dispersions 60 ~ 80%, modified silicasol 5 ~ 10%, titanium dioxide 2 ~ 5%, mica 3 ~ 5%, aqueous silicone oil 1 ~ 3%, neopelex 0.1 ~ 0.5%, alkali soluble is swollen acrylic thickener 0.5 ~ 1%, polyether-modified dimethyl siloxane 0.3 ~ 0.6%, acrylic acid copolymer sodium salt 0.1 ~ 0.5%, organic silicon modified by polyether 0.1 ~ 0.5%, balance of distilled water.
The present invention first mixes each auxiliary agent during aqueous polyurethane coating is prepared in distilled water, then to adding color stuffing to form finely dispersed mixing bottom liquid in it, mixed emulsion is well mixed with mixing bottom liquid again finally.This kind of production technology can reduce the resistance of motion of various auxiliary agents, especially wetting agent and dispersant so that they can preferably be adsorbed onto color stuffing surface, and then can greatly improve the decentralization of color stuffing, it is to avoid the problem of particle agglomeration.Aqueous protective coating is mainly made up of film forming matter, color stuffing, auxiliary agent and solvent.Wherein, film forming matter is the nucleus of protective coating, and the present invention, as film forming matter, can improve mechanical strength, strippable property and the tolerance to acid-base salt solution of coating from Aliphatic Polyester Aqueous Polyurethane Dispersions and modified silicasol compounding.The following raw material is selected in the preparation of Aliphatic Polyester Aqueous Polyurethane Dispersions：The reaction of isocyanate groups and hydroxyl is carried out with polyethylene glycol from IPDI and polypropylene glycol, the mechanical property and water resistance of film forming can be improved.In the reaction, butanone is added to reduce the viscosity of primary product.Because when the temperature of the reaction is higher than 80 DEG C, though the content of-NCO can be rapidly reached theoretical value, now side reaction is more, so easily makes unstable product quality；And when reaction is less than 58 DEG C, production efficiency can be influenceed because reaction speed is relatively slow again.Therefore, by reaction temperature control at 58 ~ 80 DEG C.From diethylenetriamine as chain extender, it can carry out chain extension to secondary product, can so improve the tensile strength of coating film.
To improve stability when alkaline silica sol is compounded with Aliphatic Polyester Aqueous Polyurethane Dispersions, the present invention has carried out surface modification treatment to alkaline silica sol.Wherein, from propyl trimethoxy silicane as silane coupler, aqueous polyurethane coating stabilization under room temperature environment can be enable to store 6 ~ 12 months and occur without gelatin phenomenon.The addition of modified silicasol can make in the nano-silica filled film to coating, and the segment of silica can constitute the network-like structure for mutually running through with the organic high molecular polymer in coating and mica, so, the pliability of organic polymer can be improved, meanwhile, coating film bulk strength and hardness can also be improved.Because the permeability of modified silicasol is fabulous, it can be penetrated into inside protected base material so that coating film is securely attached on base material.Modified silicasol can also improve the consistency of coating film, can so prevent moisture and other media from invading, and then improve the corrosion resistance of film.
Color stuffing is indispensable part in formulation for coating material, and coloring and filling effect are played in coating.Titanium dioxide is the very good Chinese white of covering power, and with good ultraviolet radiation absorption function of shielding.From mica as filler, the performances such as hardness, intensity, wearability and the base material adhesive force of coating film can be improved.Alkali soluble is swollen, and acrylic thickener can improve the viscosity of dispersion, be conducive to dispersion of the mica in system, prevent mica from sinking to luming；The denseness of coating can also be increased simultaneously, the stability of coating is improved.The base material adhesive force of adjusting coating film is capable of in the use of aqueous silicone oil, film is had preferable peeling effect.Used as wetting agent, it can reduce the surface tension of coating film to neopelex, coating film cissing phenomenon is occurred, is prevented from making application uneven because protected object is unclean with soaking base material, reduction well.Because color stuffing all has hydrophobicity, thus their less stables in water, easily reunite and sink.And pass through to add acrylic acid copolymer sodium salt, then can keep dispersiveness of the color stuffing in water.Polyether-modified dimethyl siloxane is used as levelling agent, it is possible to decrease the interfacial tension between coating and ground, improves the phenomenons such as coating is bad to shrinkage cavity that by the wetability of ground, reduction causes by ground, adhesive force.Coating is required for various artificial and mechanically actuateds in production, storage and work progress, foam is so easily caused to produce, and foam can hinder the dispersion of mica, and film coated surface is caused to form pin hole and shrinkage cavity, so as to influence the outward appearance of coating film, anti-corrosive properties and weatherability.And add the organic silicon modified by polyether can be then effectively improved above mentioned problem.
To ensure isocyanate group-NCO and being smoothed out that the hydroxyl-OH reacts, further, the mol ratio of the isocyanate group-NCO and hydroxyl-OH is 2.6 ~ 4 in the raw material of the Aliphatic Polyester Aqueous Polyurethane Dispersions:1.As-NCO/-OH ＜ 2.6, the viscosity of product can be increased, and be difficult dispersion；And as-NCO/-OH ＞ 4, the easy gel of Aliphatic Polyester Aqueous Polyurethane Dispersions reduces storage period.
To reach good neutralization, further, the addition of the triethylamine and the dihydromethyl propionic acid equimolar amounts.
It is that balance is reached between adhesive force and peel strength, further, the modified silicasol is 1 with the mass ratio of the Aliphatic Polyester Aqueous Polyurethane Dispersions:4.The consumption of modified silicasol directly affects the combination property and production cost of coating.Specifically, when the addition of modified silicasol is excessive, not only result in film and become fragile, film adhesive is excessive, be unfavorable for peeling off；The stability of coating system can be also influenceed, increases the production cost of coating.And modified silicasol consumption it is very few when, active force of the nano-particle in coating is weaker, so causes the performance improvement effect of coating unobvious.Therefore consumption of the modified silicasol in coating must be rationally appropriate.When the present invention is from the ratio, may be such that the tensile strength and elongation at break of coating film is strengthened, while moderate peel strength is also maintained, good acid and alkali-resistance salt performance.
To improve stability of the color stuffing in system, further, the addition of the acrylic acid copolymer sodium salt is the 2 ~ 4% of the titanium dioxide and mica total amount.
Further, the solid content of the ethanol and the mass ratio of the solid content of the alkaline silica sol are 1:1.Adding ethanol can slow down self condensing for silanol in propyl trimethoxy silicane, most of silanol is set to participate in the modified-reaction to alkaline silica sol, but amount of alcohol is excessive and is unfavorable for modified-reaction, thus the mass ratio of silica in ethanol and alkaline silica sol is controlled 1:1.
Further, the addition of the propyl trimethoxy silicane accounts for the 4 ~ 6% of the alkaline silica sol solid content.The consumption of propyl trimethoxy silicane must can just have good modified effect enough.If consumption is not enough, can cause that the silicone hydroxyl of alkaline silica sol particle surface is modified incomplete；If consumption is excessive, unnecessary propyl trimethoxy silicane it may happen that some side reactions and make particle aggregation or crosslinking.
Further, the operation 1）The temperature control of middle hybrid reaction is at 78 ~ 80 DEG C, and the hybrid reaction time is 100 ~ 150min.Because the reactivity of IPDI is relatively low, thus need operation 1）Reaction temperature should be higher than that 75 DEG C, along with the boiling point of butanone is 79.6 DEG C, thus can be by temperature control at 78 ~ 80 DEG C.
Effectively to control operation 1）In reaction-reaction rate of NCO group, further, the operation 1）In also comprise the following steps：During hybrid reaction, every 5 ~ 8min measurements once in first reactor-NCO group accounts for the weight/mass percentage composition of system.
The invention has the advantages that：Effective closing can be carried out to protected object using aqueous polyurethane coating obtained in the present invention to protect, and prevented protected object to be contaminated, corrode and damaged.Meanwhile, the coating also has stronger cohesive force, good strippable property, coating strength higher and stability higher.Specifically, mechanical strength, strippable property and the tolerance to acid-base salt solution of coating can be improved as film forming matter from Aliphatic Polyester Aqueous Polyurethane Dispersions and modified silicasol compounding.From mica as filler, the performances such as hardness, intensity, wearability and the base material adhesive force of coating film can be improved.The viscosity of dispersion can be improved from the swollen acrylic thickener of alkali soluble, increases the denseness of coating, improve the stability of coating.From aqueous silicone oil as remover, the base material adhesive force of energy adjusting coating film improves the rippability of film.From neopelex as wetting agent, coating can be enable film cissing phenomenon occur with soaking base material, reduction well.From acrylic acid copolymer sodium salt as dispersant, dispersiveness of the color stuffing in water can be kept.From polyether-modified dimethyl siloxane as levelling agent, it is possible to decrease the interfacial tension between coating and ground, coating is improved to by the wetability of ground.From organic silicon modified by polyether as defoamer, the generation of foam can be reduced, so as to improve the outward appearance of coating film, anti-corrosive properties and weatherability.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Embodiment 1
The preparation method of aqueous polyurethane coating, including following operation：
1）At room temperature to addition IPDI, polypropylene glycol, polyethylene glycol, dibutyl tin laurate and butanone in the first reactor, temperature is risen to 58 ~ 80 DEG C again, their-NCO% values in hybrid reaction to system in the first reactor is no longer changed, obtain primary product, it is standby；
2）By temperature control at 80 DEG C, to operation 1）Dihydromethyl propionic acid is added in the primary product of gained and 220 ~ 260min is reacted, then cools the temperature to 38 ~ 43 DEG C, addition triethylamine obtains secondary product；To adding secondary product in the second reactor for filling distilled water and secondary product is scattered in distilled water, the diethylenetriamine aqueous solution is added, Aliphatic Polyester Aqueous Polyurethane Dispersions are obtained；
3）To propyl trimethoxy silicane is added in the flask for filling ethanol, by the rotating speed stirring 5 ~ 10min of mixing of 100 ~ 200r/min, solution of silane is obtained；Rotating speed is controlled for 200 ~ 300r/min, to solution of silane is added dropwise in the 3rd reactor for filling alkaline silica sol；After completion of dropping, at a temperature of 50 ~ 65 DEG C, by the rotating speed stirring 450 ~ 500min of mixing of 250r/min, modified silicasol is obtained, it is standby；
4）At room temperature to addition operation 2 in the 4th reactor）The Aliphatic Polyester Aqueous Polyurethane Dispersions and operation 3 of gained）The modified silicasol of gained, by the rotating speed stirring 50 ~ 70min of mixing of 200 ~ 300r/min, obtains mixed emulsion, standby；
5）To adding the swollen acrylic thickener of appropriate acrylic acid copolymer sodium salt, alkali soluble and organic silicon modified by polyether in the 5th reactor for filling distilled water, by the 4 ~ 10min of rotating speed stirring mixing of 200 ~ 300r/min, add appropriate titanium dioxide, mica, by the rotating speed stirring 35 ~ 42min of mixing of 1500 ~ 1800r/min, obtain mixing bottom liquid；
6）To operation 5）Operation 4 is added in the mixing bottom liquid of gained）The mixed emulsion of gained, by the 12 ~ 22min of rotating speed stirring mixing of 350 ~ 500r/min；Appropriate neopelex, polyether-modified dimethyl siloxane, alkali soluble is swollen acrylic thickener, aqueous silicone oil, organic silicon modified by polyether are added, by the rotating speed stirring 15 ~ 20min of mixing of 200 ~ 300r/min, aqueous polyurethane coating is obtained；
The modified silicasol is obtained by the raw material of following quality proportioning：40 ~ 60 parts of alkaline silica sol, 30 ~ 50 parts of ethanol, 1 ~ 6 part of propyl trimethoxy silicane；The Aliphatic Polyester Aqueous Polyurethane Dispersions are obtained by the raw material of following quality proportioning：40 ~ 80 parts of IPDI, 25 ~ 40 parts of polypropylene glycol, 25 ~ 80 parts of polyethylene glycol, 3 ~ 10 parts of dihydromethyl propionic acid, 50 ~ 80 parts of butanone, 5 ~ 12 parts of diethylenetriamine, 3 ~ 9 parts of triethylamine, 1 ~ 3 part of dibutyl tin laurate, 40 ~ 80 parts of distilled water；The aqueous polyurethane coating is obtained by the raw material of following mass fraction：Aliphatic Polyester Aqueous Polyurethane Dispersions 60 ~ 80%, modified silicasol 5 ~ 10%, titanium dioxide 2 ~ 5%, mica 3 ~ 5%, aqueous silicone oil 1 ~ 3%, neopelex 0.1 ~ 0.5%, alkali soluble is swollen acrylic thickener 0.5 ~ 1%, polyether-modified dimethyl siloxane 0.3 ~ 0.6%, acrylic acid copolymer sodium salt 0.1 ~ 0.5%, organic silicon modified by polyether 0.1 ~ 0.5%, balance of distilled water.
The present invention first mixes each auxiliary agent during aqueous polyurethane coating is prepared in distilled water, then to adding color stuffing to form finely dispersed mixing bottom liquid in it, mixed emulsion is well mixed with mixing bottom liquid again finally.This kind of production technology can reduce the resistance of motion of various auxiliary agents, especially wetting agent and dispersant so that they can preferably be adsorbed onto color stuffing surface, and then can greatly improve the decentralization of color stuffing, it is to avoid the problem of particle agglomeration.Aqueous protective coating is mainly made up of film forming matter, color stuffing, auxiliary agent and solvent.Wherein, film forming matter is the nucleus of protective coating, and the present invention, as film forming matter, can improve mechanical strength, strippable property and the tolerance to acid-base salt solution of coating from Aliphatic Polyester Aqueous Polyurethane Dispersions and modified silicasol compounding.The following raw material is selected in the preparation of Aliphatic Polyester Aqueous Polyurethane Dispersions：The reaction of isocyanate groups and hydroxyl is carried out with polyethylene glycol from IPDI and polypropylene glycol, the mechanical property and water resistance of film forming can be improved.In the reaction, butanone is added to reduce the viscosity of primary product.Because when the temperature of the reaction is higher than 80 DEG C, though the content of-NCO can be rapidly reached theoretical value, now side reaction is more, so easily makes unstable product quality；And when reaction is less than 58 DEG C, production efficiency can be influenceed because reaction speed is relatively slow again.Therefore, by reaction temperature control at 58 ~ 80 DEG C.From diethylenetriamine as chain extender, it can carry out chain extension to secondary product, can so improve the tensile strength of coating film.
To improve stability when alkaline silica sol is compounded with Aliphatic Polyester Aqueous Polyurethane Dispersions, the present invention has carried out surface modification treatment to alkaline silica sol.Wherein, from propyl trimethoxy silicane as silane coupler, aqueous polyurethane coating stabilization under room temperature environment can be enable to store 6 ~ 12 months and occur without gelatin phenomenon.The addition of modified silicasol can make in the nano-silica filled film to coating, and the segment of silica can constitute the network-like structure for mutually running through with the organic high molecular polymer in coating and mica, so, the pliability of organic polymer can be improved, meanwhile, coating film bulk strength and hardness can also be improved.Because the permeability of modified silicasol is fabulous, it can be penetrated into inside protected base material so that coating film is securely attached on base material.Modified silicasol can also improve the consistency of coating film, can so prevent moisture and other media from invading, and then improve the corrosion resistance of film.
Color stuffing is indispensable part in formulation for coating material, and coloring and filling effect are played in coating.Titanium dioxide is the very good Chinese white of covering power, and with good ultraviolet radiation absorption function of shielding.From mica as filler, the performances such as hardness, intensity, wearability and the base material adhesive force of coating film can be improved.Alkali soluble is swollen, and acrylic thickener can improve the viscosity of dispersion, be conducive to dispersion of the mica in system, prevent mica from sinking to luming；The denseness of coating can also be increased simultaneously, the stability of coating is improved.The base material adhesive force of adjusting coating film is capable of in the use of aqueous silicone oil, film is had preferable peeling effect.Used as wetting agent, it can reduce the surface tension of coating film to neopelex, coating film cissing phenomenon is occurred, is prevented from making application uneven because protected object is unclean with soaking base material, reduction well.Because color stuffing all has hydrophobicity, thus their less stables in water, easily reunite and sink.And pass through to add acrylic acid copolymer sodium salt, then can keep dispersiveness of the color stuffing in water.Polyether-modified dimethyl siloxane is used as levelling agent, it is possible to decrease the interfacial tension between coating and ground, improves the phenomenons such as coating is bad to shrinkage cavity that by the wetability of ground, reduction causes by ground, adhesive force.Coating is required for various artificial and mechanically actuateds in production, storage and work progress, foam is so easily caused to produce, and foam can hinder the dispersion of mica, and film coated surface is caused to form pin hole and shrinkage cavity, so as to influence the outward appearance of coating film, anti-corrosive properties and weatherability.And add the organic silicon modified by polyether can be then effectively improved above mentioned problem.
To ensure isocyanate group-NCO and being smoothed out that the hydroxyl-OH reacts, it is preferable that the mol ratio of the isocyanate group-NCO and hydroxyl-OH is 2.6 ~ 4 in the raw material of the Aliphatic Polyester Aqueous Polyurethane Dispersions:1.As-NCO/-OH ＜ 2.6, the viscosity of product can be increased, and be difficult dispersion；And as-NCO/-OH ＞ 4, the easy gel of Aliphatic Polyester Aqueous Polyurethane Dispersions reduces storage period.
To reach good neutralization, it is preferable that the addition of the triethylamine and the dihydromethyl propionic acid equimolar amounts.
It is that balance is reached between adhesive force and peel strength, it is preferable that the modified silicasol is 1 with the mass ratio of the Aliphatic Polyester Aqueous Polyurethane Dispersions:4.The consumption of modified silicasol directly affects the combination property and production cost of coating.Specifically, when the addition of modified silicasol is excessive, not only result in film and become fragile, film adhesive is excessive, be unfavorable for peeling off；The stability of coating system can be also influenceed, increases the production cost of coating.And modified silicasol consumption it is very few when, active force of the nano-particle in coating is weaker, so causes the performance improvement effect of coating unobvious.Therefore consumption of the modified silicasol in coating must be rationally appropriate.When the present invention is from the ratio, may be such that the tensile strength and elongation at break of coating film is strengthened, while moderate peel strength is also maintained, good acid and alkali-resistance salt performance.
To improve stability of the color stuffing in system, it is preferable that the addition of the acrylic acid copolymer sodium salt is the 2 ~ 4% of the titanium dioxide and mica total amount.
Preferably, the solid content of the ethanol and the mass ratio of the solid content of the alkaline silica sol are 1:1.Adding ethanol can slow down self condensing for silanol in propyl trimethoxy silicane, most of silanol is set to participate in the modified-reaction to alkaline silica sol, but amount of alcohol is excessive and is unfavorable for modified-reaction, thus the mass ratio of silica in ethanol and alkaline silica sol is controlled 1:1.
Preferably, the addition of the propyl trimethoxy silicane accounts for the 4 ~ 6% of the alkaline silica sol solid content.The consumption of propyl trimethoxy silicane must can just have good modified effect enough.If consumption is not enough, can cause that the silicone hydroxyl of alkaline silica sol particle surface is modified incomplete；If consumption is excessive, unnecessary propyl trimethoxy silicane it may happen that some side reactions and make particle aggregation or crosslinking.
Preferably, the operation 1）The temperature control of middle hybrid reaction is at 78 ~ 80 DEG C, and the hybrid reaction time is 100 ~ 150min.Because the reactivity of IPDI is relatively low, thus need operation 1）Reaction temperature should be higher than that 75 DEG C, along with the boiling point of butanone is 79.6 DEG C, thus can be by temperature control at 78 ~ 80 DEG C.
Effectively to control operation 1）In reaction-reaction rate of NCO group, it is preferable that the operation 1）In also comprise the following steps：During hybrid reaction, every 5 ~ 8min measurements once in first reactor-NCO group accounts for the weight/mass percentage composition of system.
Above content is to combine the further description that specific preferred embodiment is made to the present invention, it is impossible to assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, the other embodiment drawn in the case where technical scheme is not departed from should be included within the scope of the present invention.
Claims (9)
1. the preparation method of aqueous polyurethane coating, it is characterised in that：
Including following operation：
1）At room temperature to addition IPDI, polypropylene glycol, polyethylene glycol, dibutyl tin laurate and butanone in the first reactor, temperature is risen to 58 ~ 80 DEG C again, their-NCO% values in hybrid reaction to system in the first reactor is no longer changed, obtain primary product, it is standby；
2）By temperature control at 80 DEG C, to operation 1）Dihydromethyl propionic acid is added in the primary product of gained and 220 ~ 260min is reacted, then cools the temperature to 38 ~ 43 DEG C, addition triethylamine obtains secondary product；To adding secondary product in the second reactor for filling distilled water and secondary product is scattered in distilled water, the diethylenetriamine aqueous solution is added, Aliphatic Polyester Aqueous Polyurethane Dispersions are obtained；
3）To propyl trimethoxy silicane is added in the flask for filling ethanol, by the rotating speed stirring 5 ~ 10min of mixing of 100 ~ 200r/min, solution of silane is obtained；Rotating speed is controlled for 200 ~ 300r/min, to solution of silane is added dropwise in the 3rd reactor for filling alkaline silica sol；After completion of dropping, at a temperature of 50 ~ 65 DEG C, by the rotating speed stirring 450 ~ 500min of mixing of 250r/min, modified silicasol is obtained, it is standby；
4）At room temperature to addition operation 2 in the 4th reactor）The Aliphatic Polyester Aqueous Polyurethane Dispersions and operation 3 of gained）The modified silicasol of gained, by the rotating speed stirring 50 ~ 70min of mixing of 200 ~ 300r/min, obtains mixed emulsion, standby；
5）To adding the swollen acrylic thickener of appropriate acrylic acid copolymer sodium salt, alkali soluble and organic silicon modified by polyether in the 5th reactor for filling distilled water, by the 4 ~ 10min of rotating speed stirring mixing of 200 ~ 300r/min, add appropriate titanium dioxide, mica, by the rotating speed stirring 35 ~ 42min of mixing of 1500 ~ 1800r/min, obtain mixing bottom liquid；
6）To operation 5）Operation 4 is added in the mixing bottom liquid of gained）The mixed emulsion of gained, by the 12 ~ 22min of rotating speed stirring mixing of 350 ~ 500r/min；Appropriate neopelex, polyether-modified dimethyl siloxane, alkali soluble is swollen acrylic thickener, aqueous silicone oil, organic silicon modified by polyether are added, by the rotating speed stirring 15 ~ 20min of mixing of 200 ~ 300r/min, aqueous polyurethane coating is obtained；
The modified silicasol is obtained by the raw material of following quality proportioning：40 ~ 60 parts of alkaline silica sol, 30 ~ 50 parts of ethanol, 1 ~ 6 part of propyl trimethoxy silicane；The Aliphatic Polyester Aqueous Polyurethane Dispersions are obtained by the raw material of following quality proportioning：40 ~ 80 parts of IPDI, 25 ~ 40 parts of polypropylene glycol, 25 ~ 80 parts of polyethylene glycol, 3 ~ 10 parts of dihydromethyl propionic acid, 50 ~ 80 parts of butanone, 5 ~ 12 parts of diethylenetriamine, 3 ~ 9 parts of triethylamine, 1 ~ 3 part of dibutyl tin laurate, 40 ~ 80 parts of distilled water；The aqueous polyurethane coating is obtained by the raw material of following mass fraction：Aliphatic Polyester Aqueous Polyurethane Dispersions 60 ~ 80%, modified silicasol 5 ~ 10%, titanium dioxide 2 ~ 5%, mica 3 ~ 5%, aqueous silicone oil 1 ~ 3%, neopelex 0.1 ~ 0.5%, alkali soluble is swollen acrylic thickener 0.5 ~ 1%, polyether-modified dimethyl siloxane 0.3 ~ 0.6%, acrylic acid copolymer sodium salt 0.1 ~ 0.5%, organic silicon modified by polyether 0.1 ~ 0.5%, balance of distilled water.
2. the preparation method of aqueous polyurethane coating according to claim 1, it is characterised in that：The mol ratio of the isocyanate group-NCO and hydroxyl-OH is 2.6 ~ 4 in the raw material of the Aliphatic Polyester Aqueous Polyurethane Dispersions:1.
3. the preparation method of aqueous polyurethane coating according to claim 1, it is characterised in that：The addition of the triethylamine and the dihydromethyl propionic acid equimolar amounts.
4. the preparation method of aqueous polyurethane coating according to claim 1, it is characterised in that：The modified silicasol is 1 with the mass ratio of the Aliphatic Polyester Aqueous Polyurethane Dispersions:4.
5. the preparation method of aqueous polyurethane coating according to claim 1, it is characterised in that：The addition of the acrylic acid copolymer sodium salt is the 2 ~ 4% of the titanium dioxide and mica total amount.
6. the preparation method of aqueous polyurethane coating according to claim 1, it is characterised in that：The solid content of the ethanol is 1 with the mass ratio of the solid content of the alkaline silica sol:1.
7. the preparation method of aqueous polyurethane coating according to claim 1, it is characterised in that：The addition of the propyl trimethoxy silicane accounts for the 4 ~ 6% of the alkaline silica sol solid content.
8. the preparation method of the aqueous polyurethane coating according to any one in claim 1 ~ 7, it is characterised in that：The operation 1）The temperature control of middle hybrid reaction is at 78 ~ 80 DEG C, and the hybrid reaction time is 100 ~ 150min.
9. the preparation method of aqueous polyurethane coating according to claim 8, it is characterised in that：The operation 1）In also comprise the following steps：During hybrid reaction, every 5 ~ 8min measurements once in first reactor-NCO group accounts for the weight/mass percentage composition of system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510865728.5A CN106811066A (en) | 2015-11-27 | 2015-11-27 | The preparation method of aqueous polyurethane coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510865728.5A CN106811066A (en) | 2015-11-27 | 2015-11-27 | The preparation method of aqueous polyurethane coating |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106811066A true CN106811066A (en) | 2017-06-09 |
Family
ID=59107800
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510865728.5A Pending CN106811066A (en) | 2015-11-27 | 2015-11-27 | The preparation method of aqueous polyurethane coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106811066A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107488404A (en) * | 2017-09-04 | 2017-12-19 | 上海丹韵投资管理有限公司 | A kind of automobile-used aqueous polyurethane coating and preparation method thereof |
-
2015
- 2015-11-27 CN CN201510865728.5A patent/CN106811066A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107488404A (en) * | 2017-09-04 | 2017-12-19 | 上海丹韵投资管理有限公司 | A kind of automobile-used aqueous polyurethane coating and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106811072A (en) | The preparation method of anticorrosion water-based protective film composition | |
| CN106893471A (en) | A kind of water resistance packs the preparation method of film composition | |
| CN106811081A (en) | The preparation method of aqueous Stripable paint | |
| CN106811078A (en) | Protection film composition based on modified silicasol emulsion | |
| CN106810658A (en) | The preparation method of high stability protection coating | |
| CN106810708A (en) | High intensity protects the preparation method of film composition film | |
| CN106810986A (en) | The preparation method of Aliphatic Polyester Aqueous Polyurethane Dispersions type Stripable paint | |
| CN106893474A (en) | A kind of freeze-resistant packs the preparation method of film composition | |
| CN106811094A (en) | The preparation method of the coating film containing modified silicasol | |
| CN106811066A (en) | The preparation method of aqueous polyurethane coating | |
| CN106811062A (en) | The preparation method of epoxy modified polyurethane package coating | |
| CN106811061A (en) | The preparation method of protection Stripable paint | |
| CN106893479A (en) | A kind of preparation method of powdery paints | |
| CN106893470A (en) | A kind of preparation method of fireproof coating | |
| CN106811070A (en) | Water-resistant type packs the preparation method of film composition | |
| CN106811048A (en) | The peelable protective coating of modified silicasol and polyurethane latex composite compounding | |
| CN106811075A (en) | The preparation method of modified silicasol and the peelable protective coating of polyurethane latex composite compounding formula | |
| CN106893478A (en) | The preparation method of solvent reducible coatings | |
| CN106893475A (en) | A kind of preparation method of anticorrosive paint | |
| CN106811093A (en) | The protection preparation method of coating film | |
| CN106893476A (en) | The preparation method of electrically-conducting paint | |
| CN106811071A (en) | The preparation method of the package body composition based on modified silicasol emulsion | |
| CN106893472A (en) | The preparation method of waterproof material | |
| CN106811084A (en) | The preparation method of peelable protective film composition | |
| CN106811069A (en) | The preparation method of aromatic urethane emulsion water paint |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170609 |
|
| WD01 | Invention patent application deemed withdrawn after publication |