CN106810987A - The preparation method of environment-friendly package material film - Google Patents
The preparation method of environment-friendly package material film Download PDFInfo
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- CN106810987A CN106810987A CN201510892183.7A CN201510892183A CN106810987A CN 106810987 A CN106810987 A CN 106810987A CN 201510892183 A CN201510892183 A CN 201510892183A CN 106810987 A CN106810987 A CN 106810987A
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Abstract
The invention discloses the preparation method of environment-friendly package material film, including following operation：1）At room temperature to toluene di-isocyanate(TDI) etc. is added in the first reactor, primary product is obtained；2）To the prepared acrylated aromatic polyaminoester emulsion such as addition dihydromethyl propionic acid in primary product；3）At room temperature mixed emulsion is obtained to addition Ludox and acrylated aromatic polyaminoester emulsion in the 3rd reactor；4）Obtain mixing bottom liquid to appropriate acrylic acid copolymer sodium salt etc. is added in the 4th reactor for filling distilled water；5）Environment-friendly package material is obtained to addition mixed emulsion in mixing bottom liquid；6）The plastic sheeting is cleaned air-dried, dilution environment-friendly package material；7）Environment-friendly package material is sprayed on plastic sheeting and obtains environment-friendly package material film.Effective closing can be carried out to protected object using packaging material obtained in the present invention to protect, and prevented protected object to be contaminated, corrode and damaged.
Description
Technical field
The present invention relates to decorating field, more particularly, to the preparation method of environment-friendly package material film.
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 environment-friendly package material film is provided, the performances such as tensile property to packaging material, Corrosion Protection, water vapor transmission and peel strength can be easy to test using film obtained in the present invention, so, can to coating application when coating thickness and mode of operation strong reference is provided.
The purpose of the present invention is achieved through the following technical solutions：
The preparation method of environment-friendly package material film, including following operation：
1）At room temperature to ammonium persulfate is added in the flask for filling distilled water, by the rotating speed stirring 10 ~ 20min of mixing of 100 ~ 200r/min, initiator solution is obtained, it is standby；At room temperature to addition toluene di-isocyanate(TDI), polypropylene glycol, polyethylene glycol, dibutyl tin laurate, triethylamine and butanone in the first reactor, temperature is risen to 58 ~ 70 DEG C again, their-NCO% values in hybrid reaction to system in the first reactor are made no longer to change, primary product is obtained, 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 100 ~ 130min is reacted, 58 ~ 63 DEG C are cooled the temperature to, to addition hydroxy-ethyl acrylate in the first reactor and 60 ~ 100min of reaction；38 ~ 43 DEG C are cooled the temperature to again, triethylamine is added, and obtain secondary product；At room temperature to adding secondary product in the second reactor for filling distilled water and secondary product is scattered in distilled water, ethylenediamine solution chain extension-crosslinking is added；Again to addition methyl methacrylate in the second reactor and 80 ~ 100min of reaction；Temperature is risen to 55 ~ 65 DEG C again, to dropwise addition operation 1 in the second reactor）The initiator solution of gained, 100 ~ 120min of hybrid reaction, acrylated aromatic polyaminoester emulsion is obtained, it is standby；
3）At room temperature to addition Ludox and operation 2 in the 3rd reactor）The acrylated aromatic polyaminoester emulsion of gained, by the rotating speed stirring 50 ~ 70min of mixing of 200 ~ 300r/min, obtains mixed emulsion, standby；
4）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；
5）To operation 4）Operation 3 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 15 ~ 20min of rotating speed stirring mixing of 200 ~ 300r/min, environment-friendly package material is obtained, it is standby；
6）A plastic sheeting is taken, the film is cleaned with acetone, then the film is placed on air-dried 1d at room temperature, it is standby；Take appropriate operation 5）The environment-friendly package material of gained, and it is diluted with deionized water, it is standby；
7）By operation 6）The environment-friendly package material for diluting treatment is sprayed at operation 6）On handled plastic sheeting, holding wet-film thickness is 10 ~ 30um, then the plastic sheeting after film is air-dried into 3d at room temperature, repeats aforementioned operation 3 times, obtains environment-friendly package material film；
The acrylated aromatic polyaminoester 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 ~ 20 parts of methyl methacrylate, 3 ~ 8 parts of hydroxy-ethyl acrylate, 0.5 ~ 2 part of ammonium persulfate, 50 ~ 80 parts of butanone, 5 ~ 12 parts of ethylenediamine, 3 ~ 11 parts of triethylamine, 1 ~ 3 part of dibutyl tin laurate, 40 ~ 80 parts of distilled water；The environment-friendly package material is obtained by the raw material of following mass fraction：Acrylated aromatic polyaminoester 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 environment-friendly package material 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.Operation 7）The film of gained can be easy to the performances such as tensile property to packaging material, Corrosion Protection, water vapor transmission and peel strength to test, so, can to coating application when coating thickness and mode of operation strong reference is provided.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 acrylated aromatic polyaminoester emulsion and Ludox compounding.The following raw material is selected in the preparation of acrylated aromatic polyaminoester 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 hydroxy-ethyl acrylate, water resistance, alkali resistance, hardness and the photostability of coating film can be so improved on the premise of the original toughness of polyurethane and elasticity is kept.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 ethylenediamine 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 acrylated aromatic polyaminoester 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 easy gel of acrylated aromatic polyaminoester 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 acrylated aromatic polyaminoester 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 1）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 1）Reaction temperature can be controlled in 68 ~ 70 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 3 ~ 5min measurements once in first reactor-NCO group accounts for the weight/mass percentage composition of system.
The invention has the advantages that：The performances such as tensile property to environment-friendly package material, Corrosion Protection, water vapor transmission and peel strength can be easy to test using film obtained in the present invention, so, can to coating application when coating thickness and mode of operation strong reference is provided.Obtained packaging material of the invention can carry out effective closing protection to protected object, prevent protected object to be contaminated, corrode and damage.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 acrylated aromatic polyaminoester 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 environment-friendly package material film, including following operation：
1）At room temperature to ammonium persulfate is added in the flask for filling distilled water, by the rotating speed stirring 10 ~ 20min of mixing of 100 ~ 200r/min, initiator solution is obtained, it is standby；At room temperature to addition toluene di-isocyanate(TDI), polypropylene glycol, polyethylene glycol, dibutyl tin laurate, triethylamine and butanone in the first reactor, temperature is risen to 58 ~ 70 DEG C again, their-NCO% values in hybrid reaction to system in the first reactor are made no longer to change, primary product is obtained, 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 100 ~ 130min is reacted, 58 ~ 63 DEG C are cooled the temperature to, to addition hydroxy-ethyl acrylate in the first reactor and 60 ~ 100min of reaction；38 ~ 43 DEG C are cooled the temperature to again, triethylamine is added, and obtain secondary product；At room temperature to adding secondary product in the second reactor for filling distilled water and secondary product is scattered in distilled water, ethylenediamine solution chain extension-crosslinking is added；Again to addition methyl methacrylate in the second reactor and 80 ~ 100min of reaction；Temperature is risen to 55 ~ 65 DEG C again, to dropwise addition operation 1 in the second reactor）The initiator solution of gained, 100 ~ 120min of hybrid reaction, acrylated aromatic polyaminoester emulsion is obtained, it is standby；
3）At room temperature to addition Ludox and operation 2 in the 3rd reactor）The acrylated aromatic polyaminoester emulsion of gained, by the rotating speed stirring 50 ~ 70min of mixing of 200 ~ 300r/min, obtains mixed emulsion, standby；
4）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；
5）To operation 4）Operation 3 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 15 ~ 20min of rotating speed stirring mixing of 200 ~ 300r/min, environment-friendly package material is obtained, it is standby；
6）A plastic sheeting is taken, the film is cleaned with acetone, then the film is placed on air-dried 1d at room temperature, it is standby；Take appropriate operation 5）The environment-friendly package material of gained, and it is diluted with deionized water, it is standby；
7）By operation 6）The environment-friendly package material for diluting treatment is sprayed at operation 6）On handled plastic sheeting, holding wet-film thickness is 10 ~ 30um, then the plastic sheeting after film is air-dried into 3d at room temperature, repeats aforementioned operation 3 times, obtains environment-friendly package material film；
The acrylated aromatic polyaminoester 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 ~ 20 parts of methyl methacrylate, 3 ~ 8 parts of hydroxy-ethyl acrylate, 0.5 ~ 2 part of ammonium persulfate, 50 ~ 80 parts of butanone, 5 ~ 12 parts of ethylenediamine, 3 ~ 11 parts of triethylamine, 1 ~ 3 part of dibutyl tin laurate, 40 ~ 80 parts of distilled water；The environment-friendly package material is obtained by the raw material of following mass fraction：Acrylated aromatic polyaminoester 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 environment-friendly package material 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.The performances such as tensile property to environment-friendly package material, Corrosion Protection, water vapor transmission and peel strength can be easy to test using film obtained in the present invention, so, can to coating application when coating thickness and mode of operation strong reference is provided.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 acrylated aromatic polyaminoester emulsion and Ludox compounding.The following raw material is selected in the preparation of acrylated aromatic polyaminoester 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 hydroxy-ethyl acrylate, water resistance, alkali resistance, hardness and the photostability of coating film can be so improved on the premise of the original toughness of polyurethane and elasticity is kept.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 ethylenediamine 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 acrylated aromatic polyaminoester 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 easy gel of acrylated aromatic polyaminoester 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 acrylated aromatic polyaminoester 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 1）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 1）Reaction temperature can be controlled in 68 ~ 70 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 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 environment-friendly package material film, it is characterised in that：
Including following operation：
1）At room temperature to ammonium persulfate is added in the flask for filling distilled water, by the rotating speed stirring 10 ~ 20min of mixing of 100 ~ 200r/min, initiator solution is obtained, it is standby；At room temperature to addition toluene di-isocyanate(TDI), polypropylene glycol, polyethylene glycol, dibutyl tin laurate, triethylamine and butanone in the first reactor, temperature is risen to 58 ~ 70 DEG C again, their-NCO% values in hybrid reaction to system in the first reactor are made no longer to change, primary product is obtained, 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 100 ~ 130min is reacted, 58 ~ 63 DEG C are cooled the temperature to, to addition hydroxy-ethyl acrylate in the first reactor and 60 ~ 100min of reaction；38 ~ 43 DEG C are cooled the temperature to again, triethylamine is added, and obtain secondary product；At room temperature to adding secondary product in the second reactor for filling distilled water and secondary product is scattered in distilled water, ethylenediamine solution chain extension-crosslinking is added；Again to addition methyl methacrylate in the second reactor and 80 ~ 100min of reaction；Temperature is risen to 55 ~ 65 DEG C again, to dropwise addition operation 1 in the second reactor）The initiator solution of gained, 100 ~ 120min of hybrid reaction, acrylated aromatic polyaminoester emulsion is obtained, it is standby；
3）At room temperature to addition Ludox and operation 2 in the 3rd reactor）The acrylated aromatic polyaminoester emulsion of gained, by the rotating speed stirring 50 ~ 70min of mixing of 200 ~ 300r/min, obtains mixed emulsion, standby；
4）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；
5）To operation 4）Operation 3 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 15 ~ 20min of rotating speed stirring mixing of 200 ~ 300r/min, environment-friendly package material is obtained, it is standby；
6）A plastic sheeting is taken, the film is cleaned with acetone, then the film is placed on air-dried 1d at room temperature, it is standby；Take appropriate operation 5）The environment-friendly package material of gained, and it is diluted with deionized water, it is standby；
7）By operation 6）The environment-friendly package material for diluting treatment is sprayed at operation 6）On handled plastic sheeting, holding wet-film thickness is 10 ~ 30um, then the plastic sheeting after film is air-dried into 3d at room temperature, repeats aforementioned operation 3 times, obtains environment-friendly package material film；
The acrylated aromatic polyaminoester 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 ~ 20 parts of methyl methacrylate, 3 ~ 8 parts of hydroxy-ethyl acrylate, 0.5 ~ 2 part of ammonium persulfate, 50 ~ 80 parts of butanone, 5 ~ 12 parts of ethylenediamine, 3 ~ 11 parts of triethylamine, 1 ~ 3 part of dibutyl tin laurate, 40 ~ 80 parts of distilled water；The environment-friendly package material is obtained by the raw material of following mass fraction：Acrylated aromatic polyaminoester 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 environment-friendly package material film 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 acrylated aromatic polyaminoester emulsion:1.
3. the preparation method of environment-friendly package material film 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 environment-friendly package material film according to claim 1, it is characterised in that：The Ludox is 1 with the mass ratio of the acrylated aromatic polyaminoester emulsion:4.
5. the preparation method of environment-friendly package material film 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 environment-friendly package material film according to any one in claim 1 ~ 5, it is characterised in that：The operation 1）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 environment-friendly package material film according to claim 6, it is characterised in that：The operation 1）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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| CN201510892183.7A Pending CN106810987A (en) | 2015-11-27 | 2015-11-27 | The preparation method of environment-friendly package material film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108587125A (en) * | 2018-05-17 | 2018-09-28 | 合肥浦尔菲电线科技有限公司 | A kind of environment-friendly package material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587125A (en) * | 2018-05-17 | 2018-09-28 | 合肥浦尔菲电线科技有限公司 | A kind of environment-friendly package material and preparation method thereof |
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