CN106811069A - The preparation method of aromatic urethane emulsion water paint - Google Patents
The preparation method of aromatic urethane emulsion water paint Download PDFInfo
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- CN106811069A CN106811069A CN201510891038.7A CN201510891038A CN106811069A CN 106811069 A CN106811069 A CN 106811069A CN 201510891038 A CN201510891038 A CN 201510891038A CN 106811069 A CN106811069 A CN 106811069A
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Abstract
The invention discloses the preparation method of aromatic urethane emulsion water paint, including following operation：1）Epoxy resin-butanone solution is obtained；Raw material is carried out to dehydrate treatment；2）To toluene di-isocyanate(TDI) etc. is added in the first reactor, primary product is obtained；3）To dihydromethyl propionic acid is added in primary product, triethylamine is added, epoxide modified aromatic urethane emulsion is obtained；4）At room temperature to Ludox and epoxide modified aromatic urethane emulsion is added in the 3rd reactor, mixed emulsion is obtained, it is standby；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, aromatic urethane emulsion water paint is obtained.There is excellent water resistance, stability higher, stronger cohesive force, good strippable property and coating strength higher using coating obtained in the present invention.
Description
Technical field
The present invention relates to decorating field, more particularly, to the preparation method of aromatic urethane emulsion water paint.
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 aromatic urethane emulsion water paint 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 water resistance is strong, stability is high, strippable property good, coating strength is high and cohesive force is strong.
The purpose of the present invention is achieved through the following technical solutions：
The preparation method of aromatic urethane emulsion water paint, including following operation：
1）To butanone is added in the flask for filling epoxy resin, by the rotating speed stirring 10 ~ 30min of mixing of 150 ~ 200r/min, epoxy resin-butanone solution is obtained, it is standby；Raw material polypropylene glycol is put into drying box and is dehydrated 450 ~ 500min, drying temperature is controlled at 110 ~ 125 DEG C, standby；Raw material dihydromethyl propionic acid is put into baking oven and dries 100 ~ 150 min, drying temperature is controlled at 110 ~ 125 DEG C, standby；Raw material triethylamine and butanone are carried out into dewater treatment 5 ~ 7d with molecular sieve, it is standby；
2）At room temperature in the first reactor add toluene di-isocyanate(TDI), dibutyl tin laurate, through operation 1）The polypropylene glycol of dewater treatment, polyethylene glycol, triethylamine and butanone, then temperature is risen to 58 ~ 70 DEG C, their-NCO% values in hybrid reaction to system in the first reactor is no longer changed, primary product is obtained, it is standby；
3）By temperature control at 80 DEG C, to operation 2）Added through operation 1 in the primary product of gained）The dihydromethyl propionic acid of dried process simultaneously reacts 100 ~ 130min, adds operation 1）Epoxy resin-the butanone solution of gained simultaneously reacts 100 ~ 130min；38 ~ 43 DEG C are cooled the temperature to again, triethylamine is added, and obtain 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, epoxide modified aromatic urethane emulsion is obtained, it is standby；
4）At room temperature to addition Ludox and operation 3 in the 3rd reactor）The epoxide modified aromatic urethane emulsion 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 4th reactor for filling distilled water, by the 4 ~ 10min of rotating speed stirring mixing of 200 ~ 300r/min, add appropriate talcum powder, by the 35 ~ 42min of rotating speed stirring mixing of 1500 ~ 1800r/min, obtain mixing bottom liquid, it is standby；
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；Add appropriate acrylate copolymer ammonium salt solution, polyether polyester azo polyether polyeste, alkali soluble is swollen acrylic thickener, silicone emulsion, organic silicon modified by polyether, by the rotating speed stirring 15 ~ 20min of mixing of 200 ~ 300r/min, aromatic urethane emulsion water paint is obtained；
The epoxide modified aromatic urethane emulsion is obtained by the raw material of following quality proportioning：40 ~ 80 parts of toluene di-isocyanate(TDI), 25 ~ 40 parts of polypropylene glycol, 25 ~ 60 parts of polyethylene glycol, 3 ~ 10 parts of dihydromethyl propionic acid, 5 ~ 12 parts of epoxy resin, 50 ~ 80 parts of butanone, 4 ~ 10 parts of diethylenetriamine, 3 ~ 11 parts of triethylamine, 1 ~ 3 part of dibutyl tin laurate, 40 ~ 80 parts of distilled water；The aromatic urethane emulsion water paint is obtained by the raw material of following mass fraction：Epoxide modified aromatic urethane emulsion 60 ~ 80%, Ludox 5 ~ 10%, talcum powder 3 ~ 8%, silicone emulsion 1 ~ 3%, acrylate copolymer ammonium salt solution 0.1 ~ 0.5%, alkali soluble is swollen acrylic thickener 0.5 ~ 1%, polyether polyester azo polyether polyeste 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 aromatic urethane emulsion water paint is prepared in distilled water, then to adding filler 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 filler surface, and then can greatly improve the decentralization of filler, it is to avoid the problem of particle agglomeration.During epoxide modified aromatic urethane emulsion is prepared, to avoid-NCO group and the aqueous generation side reaction of each raw material, then part material carried out before synthesis dehydrating treatment.Aqueous protective coating is mainly made up of film forming matter, filler, auxiliary agent and solvent.Wherein, film forming matter is the nucleus of protective coating, and the present invention, as film forming matter, can improve stability, strippable property, mechanical strength and the tolerance to acid-base salt solution of coating from epoxide modified aromatic urethane emulsion and Ludox compounding.The following raw material is selected in the preparation of epoxide modified aromatic urethane emulsion：The reaction of isocyanate groups and hydroxyl is carried out from toluene di-isocyanate(TDI) and polypropylene glycol and polyethylene glycol, and polyurethane is modified from epoxy resin, can so improve the water resistance and mechanical property of coating film.Epoxy resin can select E-44.In the reaction, butanone is added to reduce the viscosity of primary product.Because when the temperature of the reaction is higher than 70 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 ~ 70 DEG C.Relatively it is used alone for dibutyl tin laurate, reaction rate can be significantly improved as catalyst from dibutyl tin laurate and triethylamine compounding, offsets the adverse effect of solvent effect.From diethylenetriamine as chain extender, it can carry out chain extension to secondary product, can so improve the tensile strength of coating film.The addition of Ludox 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 talcum powder, so, the pliability of organic polymer can be improved, meanwhile, coating film bulk strength and hardness can also be improved.Because the permeability of Ludox is fabulous, it can be penetrated into inside protected base material so that coating film is securely attached on base material.Ludox 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.
Filler is indispensable part in formulation for coating material, and filling effect is played in coating.From talcum powder as filler, paint coatings can be prevented to be cracked, improve levelability, washability, water resistance of coating etc..Alkali soluble is swollen, and acrylic thickener can improve the viscosity of dispersion, be conducive to dispersion of the talcum powder in system, prevent talcum powder 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 silicone emulsion, film is had preferable peeling effect.Used as wetting agent, it can reduce the surface tension of coating film to acrylate copolymer ammonium salt solution, coating film cissing phenomenon is occurred, is prevented from making application uneven because protected object is unclean with soaking base material, reduction well.Because filler 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 filler in water.Polyether polyester azo polyether polyeste 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 talcum powder, 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 2.2 ~ 3.6 in the raw material of the epoxide modified aromatic urethane emulsion:1.As-NCO/-OH ＜ 2.2, the viscosity of product can be increased, and be difficult dispersion；And as-NCO/-OH ＞ 3.6, the epoxide modified easy gel of aromatic urethane emulsion 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 Ludox is 1 with the mass ratio of the epoxide modified aromatic urethane emulsion:4.The consumption of Ludox directly affects the combination property and production cost of coating.Specifically, when the addition of Ludox 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 Ludox 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 Ludox 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 filler in system, further, the addition of the acrylic acid copolymer sodium salt is the 2 ~ 4% of the talcum powder addition.
Further, the operation 2）The temperature control of middle hybrid reaction is at 68 ~ 70 DEG C, and the hybrid reaction time is 50 ~ 75min.Because the reactivity of toluene di-isocyanate(TDI) is higher, thus operation 2）Reaction temperature can be controlled in 68 ~ 70 DEG C.
Effectively to control operation 2）In reaction-reaction rate of NCO group, further, the operation 2）In also comprise the following steps：During hybrid reaction, every 3 ~ 5min 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 aromatic urethane emulsion water paint obtained in the present invention to protect, and prevented protected object to be contaminated, corrode and damaged.Meanwhile, the coating also has excellent water resistance, stability higher, stronger cohesive force, good strippable property and coating strength higher.Specifically, mechanical strength, strippable property and the tolerance to acid-base salt solution of coating can be improved as film forming matter from epoxide modified aromatic urethane emulsion and Ludox compounding.From talcum powder as filler, the performances such as hardness, intensity, wearability and the base material adhesive force of coating film can be improved.Reaction rate can be significantly improved as catalyst from dibutyl tin laurate and triethylamine compounding, the adverse effect of solvent effect is offset.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 silicone emulsion as remover, the base material adhesive force of energy adjusting coating film improves the rippability of film.From acrylate copolymer ammonium salt solution 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 filler in water can be kept.From polyether polyester azo polyether polyeste 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 aromatic urethane emulsion water paint, including following operation：
1）To butanone is added in the flask for filling epoxy resin, by the rotating speed stirring 10 ~ 30min of mixing of 150 ~ 200r/min, epoxy resin-butanone solution is obtained, it is standby；Raw material polypropylene glycol is put into drying box and is dehydrated 450 ~ 500min, drying temperature is controlled at 110 ~ 125 DEG C, standby；Raw material dihydromethyl propionic acid is put into baking oven and dries 100 ~ 150 min, drying temperature is controlled at 110 ~ 125 DEG C, standby；Raw material triethylamine and butanone are carried out into dewater treatment 5 ~ 7d with molecular sieve, it is standby；
2）At room temperature in the first reactor add toluene di-isocyanate(TDI), dibutyl tin laurate, through operation 1）The polypropylene glycol of dewater treatment, polyethylene glycol, triethylamine and butanone, then temperature is risen to 58 ~ 70 DEG C, their-NCO% values in hybrid reaction to system in the first reactor is no longer changed, primary product is obtained, it is standby；
3）By temperature control at 80 DEG C, to operation 2）Added through operation 1 in the primary product of gained）The dihydromethyl propionic acid of dried process simultaneously reacts 100 ~ 130min, adds operation 1）Epoxy resin-the butanone solution of gained simultaneously reacts 100 ~ 130min；38 ~ 43 DEG C are cooled the temperature to again, triethylamine is added, and obtain 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, epoxide modified aromatic urethane emulsion is obtained, it is standby；
4）At room temperature to addition Ludox and operation 3 in the 3rd reactor）The epoxide modified aromatic urethane emulsion 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 4th reactor for filling distilled water, by the 4 ~ 10min of rotating speed stirring mixing of 200 ~ 300r/min, add appropriate talcum powder, by the 35 ~ 42min of rotating speed stirring mixing of 1500 ~ 1800r/min, obtain mixing bottom liquid, it is standby；
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；Add appropriate acrylate copolymer ammonium salt solution, polyether polyester azo polyether polyeste, alkali soluble is swollen acrylic thickener, silicone emulsion, organic silicon modified by polyether, by the rotating speed stirring 15 ~ 20min of mixing of 200 ~ 300r/min, aromatic urethane emulsion water paint is obtained；
The epoxide modified aromatic urethane emulsion is obtained by the raw material of following quality proportioning：40 ~ 80 parts of toluene di-isocyanate(TDI), 25 ~ 40 parts of polypropylene glycol, 25 ~ 60 parts of polyethylene glycol, 3 ~ 10 parts of dihydromethyl propionic acid, 5 ~ 12 parts of epoxy resin, 50 ~ 80 parts of butanone, 4 ~ 10 parts of diethylenetriamine, 3 ~ 11 parts of triethylamine, 1 ~ 3 part of dibutyl tin laurate, 40 ~ 80 parts of distilled water；The aromatic urethane emulsion water paint is obtained by the raw material of following mass fraction：Epoxide modified aromatic urethane emulsion 60 ~ 80%, Ludox 5 ~ 10%, talcum powder 3 ~ 8%, silicone emulsion 1 ~ 3%, acrylate copolymer ammonium salt solution 0.1 ~ 0.5%, alkali soluble is swollen acrylic thickener 0.5 ~ 1%, polyether polyester azo polyether polyeste 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 aromatic urethane emulsion water paint is prepared in distilled water, then to adding filler 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 filler surface, and then can greatly improve the decentralization of filler, it is to avoid the problem of particle agglomeration.During epoxide modified aromatic urethane emulsion is prepared, to avoid-NCO group and the aqueous generation side reaction of each raw material, then part material carried out before synthesis dehydrating treatment.Aqueous protective coating is mainly made up of film forming matter, filler, auxiliary agent and solvent.Wherein, film forming matter is the nucleus of protective coating, and the present invention, as film forming matter, can improve stability, strippable property, mechanical strength and the tolerance to acid-base salt solution of coating from epoxide modified aromatic urethane emulsion and Ludox compounding.The following raw material is selected in the preparation of epoxide modified aromatic urethane emulsion：The reaction of isocyanate groups and hydroxyl is carried out from toluene di-isocyanate(TDI) and polypropylene glycol and polyethylene glycol, and polyurethane is modified from epoxy resin, can so improve the water resistance and mechanical property of coating film.Epoxy resin can select E-44.In the reaction, butanone is added to reduce the viscosity of primary product.Because when the temperature of the reaction is higher than 70 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 ~ 70 DEG C.Relatively it is used alone for dibutyl tin laurate, reaction rate can be significantly improved as catalyst from dibutyl tin laurate and triethylamine compounding, offsets the adverse effect of solvent effect.From diethylenetriamine as chain extender, it can carry out chain extension to secondary product, can so improve the tensile strength of coating film.The addition of Ludox 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 talcum powder, so, the pliability of organic polymer can be improved, meanwhile, coating film bulk strength and hardness can also be improved.Because the permeability of Ludox is fabulous, it can be penetrated into inside protected base material so that coating film is securely attached on base material.Ludox 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.
Filler is indispensable part in formulation for coating material, and filling effect is played in coating.From talcum powder as filler, paint coatings can be prevented to be cracked, improve levelability, washability, water resistance of coating etc..Alkali soluble is swollen, and acrylic thickener can improve the viscosity of dispersion, be conducive to dispersion of the talcum powder in system, prevent talcum powder 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 silicone emulsion, film is had preferable peeling effect.Used as wetting agent, it can reduce the surface tension of coating film to acrylate copolymer ammonium salt solution, coating film cissing phenomenon is occurred, is prevented from making application uneven because protected object is unclean with soaking base material, reduction well.Because filler 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 filler in water.Polyether polyester azo polyether polyeste 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 talcum powder, 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 2.2 ~ 3.6 in the raw material of the epoxide modified aromatic urethane emulsion:1.As-NCO/-OH ＜ 2.2, the viscosity of product can be increased, and be difficult dispersion；And as-NCO/-OH ＞ 3.6, the epoxide modified easy gel of aromatic urethane emulsion 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 Ludox is 1 with the mass ratio of the epoxide modified aromatic urethane emulsion:4.The consumption of Ludox directly affects the combination property and production cost of coating.Specifically, when the addition of Ludox 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 Ludox 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 Ludox 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 filler in system, it is preferable that the addition of the acrylic acid copolymer sodium salt is the 2 ~ 4% of the talcum powder addition.
Preferably, the operation 2）The temperature control of middle hybrid reaction is at 68 ~ 70 DEG C, and the hybrid reaction time is 50 ~ 75min.Because the reactivity of toluene di-isocyanate(TDI) is higher, thus operation 2）Reaction temperature can be controlled in 68 ~ 70 DEG C.
Effectively to control operation 2）In reaction-reaction rate of NCO group, it is preferable that the operation 2）In also comprise the following steps：During hybrid reaction, every 3 ~ 5min 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 (7)
1. the preparation method of aromatic urethane emulsion water paint, it is characterised in that：
Including following operation：
1）To butanone is added in the flask for filling epoxy resin, by the rotating speed stirring 10 ~ 30min of mixing of 150 ~ 200r/min, epoxy resin-butanone solution is obtained, it is standby；Raw material polypropylene glycol is put into drying box and is dehydrated 450 ~ 500min, drying temperature is controlled at 110 ~ 125 DEG C, standby；Raw material dihydromethyl propionic acid is put into baking oven and dries 100 ~ 150 min, drying temperature is controlled at 110 ~ 125 DEG C, standby；Raw material triethylamine and butanone are carried out into dewater treatment 5 ~ 7d with molecular sieve, it is standby；
2）At room temperature in the first reactor add toluene di-isocyanate(TDI), dibutyl tin laurate, through operation 1）The polypropylene glycol of dewater treatment, polyethylene glycol, triethylamine and butanone, then temperature is risen to 58 ~ 70 DEG C, their-NCO% values in hybrid reaction to system in the first reactor is no longer changed, primary product is obtained, it is standby；
3）By temperature control at 80 DEG C, to operation 2）Added through operation 1 in the primary product of gained）The dihydromethyl propionic acid of dried process simultaneously reacts 100 ~ 130min, adds operation 1）Epoxy resin-the butanone solution of gained simultaneously reacts 100 ~ 130min；38 ~ 43 DEG C are cooled the temperature to again, triethylamine is added, and obtain 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, epoxide modified aromatic urethane emulsion is obtained, it is standby；
4）At room temperature to addition Ludox and operation 3 in the 3rd reactor）The epoxide modified aromatic urethane emulsion 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 4th reactor for filling distilled water, by the 4 ~ 10min of rotating speed stirring mixing of 200 ~ 300r/min, add appropriate talcum powder, by the 35 ~ 42min of rotating speed stirring mixing of 1500 ~ 1800r/min, obtain mixing bottom liquid, it is standby；
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；Add appropriate acrylate copolymer ammonium salt solution, polyether polyester azo polyether polyeste, alkali soluble is swollen acrylic thickener, silicone emulsion, organic silicon modified by polyether, by the rotating speed stirring 15 ~ 20min of mixing of 200 ~ 300r/min, aromatic urethane emulsion water paint is obtained；
The epoxide modified aromatic urethane emulsion is obtained by the raw material of following quality proportioning：40 ~ 80 parts of toluene di-isocyanate(TDI), 25 ~ 40 parts of polypropylene glycol, 25 ~ 60 parts of polyethylene glycol, 3 ~ 10 parts of dihydromethyl propionic acid, 5 ~ 12 parts of epoxy resin, 50 ~ 80 parts of butanone, 4 ~ 10 parts of diethylenetriamine, 3 ~ 11 parts of triethylamine, 1 ~ 3 part of dibutyl tin laurate, 40 ~ 80 parts of distilled water；The aromatic urethane emulsion water paint is obtained by the raw material of following mass fraction：Epoxide modified aromatic urethane emulsion 60 ~ 80%, Ludox 5 ~ 10%, talcum powder 3 ~ 8%, silicone emulsion 1 ~ 3%, acrylate copolymer ammonium salt solution 0.1 ~ 0.5%, alkali soluble is swollen acrylic thickener 0.5 ~ 1%, polyether polyester azo polyether polyeste 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 aromatic urethane emulsion water paint according to claim 1, it is characterised in that：The mol ratio of the isocyanate group-NCO and hydroxyl-OH is 2.2 ~ 3.6 in the raw material of the epoxide modified aromatic urethane emulsion:1.
3. the preparation method of aromatic urethane emulsion water paint 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 aromatic urethane emulsion water paint according to claim 1, it is characterised in that：The Ludox is 1 with the mass ratio of the epoxide modified aromatic urethane emulsion:4.
5. the preparation method of aromatic urethane emulsion water paint according to claim 1, it is characterised in that：The addition of the acrylic acid copolymer sodium salt is the 2 ~ 4% of the talcum powder addition.
6. the preparation method of the aromatic urethane emulsion water paint according to any one in claim 1 ~ 5, it is characterised in that：The operation 2）The temperature control of middle hybrid reaction is at 68 ~ 70 DEG C, and the hybrid reaction time is 50 ~ 75min.
7. the preparation method of aromatic urethane emulsion water paint according to claim 6, it is characterised in that：The operation 2）In also comprise the following steps：During hybrid reaction, every 3 ~ 5min measurements once in first reactor-NCO group accounts for the weight/mass percentage composition of system.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113801271A (en) * | 2021-08-18 | 2021-12-17 | 华南理工大学 | Silica sol modified waterborne polyurethane acrylate composite emulsion and preparation thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113801271A (en) * | 2021-08-18 | 2021-12-17 | 华南理工大学 | Silica sol modified waterborne polyurethane acrylate composite emulsion and preparation thereof |
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Application publication date: 20170609 |