CN109762128A - A kind of preparation method and applications of aqueous polyurethane transfer latex solution - Google Patents
A kind of preparation method and applications of aqueous polyurethane transfer latex solution Download PDFInfo
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- CN109762128A CN109762128A CN201811595998.9A CN201811595998A CN109762128A CN 109762128 A CN109762128 A CN 109762128A CN 201811595998 A CN201811595998 A CN 201811595998A CN 109762128 A CN109762128 A CN 109762128A
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- aqueous polyurethane
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Abstract
The invention discloses a kind of preparation method and applications of aqueous polyurethane transfer latex solution, this method is using diisocyanate, polycaprolactone polyol or/and polytetramethylene ether diol as raw material, dibutyl tin dilaurate is catalyst, and acetone is that reaction medium obtains base polyurethane prepolymer for use as；Dihydromethyl propionic acid is added, the aqueous solution that addition ethylenediamine under triethylamine neutralization reaction generation salt, then high speed shear is added is emulsified chain extension again；Finally, removing acetone under reduced pressure, aqueous polyurethane emulsion is obtained.Reaction process of the present invention due to no added crosslinking agent, save production cost, solve the problems, such as that reaction is uneven, not easy to control simultaneously, obtained aqueous polyurethane emulsion has preferable stability, its glue film has preferable mechanical property, and the aqueous polyurethane emulsion bond properties compound with the transfer of art paper, Hongta Huang core paper, Yi Gesende paper, Chinese paper and each germplasm bottom art post paperboard for transfer aluminum plated film, transfer laser film is preferable.
Description
Technical field
The present invention relates to emulsion technology field, in particular to the preparation method of a kind of aqueous polyurethane transfer latex solution and its
Using.
Background technique
Aqueous polyurethane is to replace organic solvent as the new polyurethane system of decentralized medium using water, and also referred to as water dispersion is poly-
Urethane, aqueous polyurethane or water-based polyurethane.Aqueous polyurethane takes water as a solvent, pollution-free, safe and reliable, mechanical performance is excellent
Good, the advantages that compatibility is good, easily modified.The Water-borne modification of polyurethane resin gradually replaces solvent type, becomes polyurethane industrial
The important directions of development.Aqueous polyurethane can be widely applied to coating, adhesive, fabric coating and finishing agent, leather finishing agent,
Sheet surface treating agent and fiber surface treatment agent.Currently, synthesized using polycaprolactone polyol and polyether polyol as soft segment
Aqueous polyurethane emulsion, but its bond properties of the aqueous polyurethane of preparation is bad.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and applications of aqueous polyurethane emulsion, and this method is with two
Isocyanates, polycaprolactone polyol, polytetramethylene ether diol, dihydromethyl propionic acid are raw material preparing performed polymer, are added three
Ethamine carries out neutralization reaction and generates salt, and the aqueous solution that ethylenediamine is added carries out emulsification chain extension, and aqueous polyurethane emulsion is made, has
Reaction is uniformly easy to control, and the degree of cross linking is moderate, and stability is good, and mechanics performance of latex film is good, the good feature of bond properties.
To achieve the above object, a kind of the technical solution used in the present invention: preparation of aqueous polyurethane transfer latex solution
Method, comprising the following steps:
It 1) is original with diisocyanate, polycaprolactone polyol or/and polytetramethylene ether diol, dihydromethyl propionic acid
Material, dibutyl tin dilaurate are catalyst, and acetone is that reaction medium obtains base polyurethane prepolymer for use as；
2) aqueous solution that addition ethylenediamine under triethylamine neutralization reaction generation salt, then high speed shear is added is emulsified to be expanded again
Chain；
3) finally, removing acetone under reduced pressure, aqueous polyurethane emulsion is obtained.
Polyurethane is that the polymer in macromolecular main chain containing carbamate groups is known as polyurethanes.Polyurethane
It is divided into polyester polyurethane and polyether polyurethane two major classes.Polyester-type is using diisocyanate and hydroxyl telechelic polyester as raw material system
Standby polyurethane.Polyether polyurethane is the polyurethane prepared using diisocyanate and end hydroxy polyether as raw material.The present invention with
Diisocyanate and polycaprolactone polyol, polytetramethylene ether diol raw material prepare polyurethane, and polyester polyurethane can be made
And/or polyether polyurethane.
Polyaminoester emulsion prepared by the present invention since the group contained in polyurethane macromolecular is all highly polar group, and
Also contain polyethers or polyester flexible segment in macromolecular, so that polyurethane has the following characteristics that higher mechanical strength and oxidation
Stability；Flexibility with higher and resilience；With excellent oil resistivity, solvent resistance, water resistance and fire resistance.Due to
Polyurethane has many excellent performances, so its tool has been widely used.Aqueous polyurethane emulsion application prepared by the present invention
In PET class compound adhesive, paper and transfer adhesive, compound adhesive, the Paper Coating of aluminium coated etc. turn especially suitable for high-grade paper and aluminium coated
Divert from one use to another glue.The main product that improves is to paper and aluminium foil high adhesion force and folding resistance.
Preferably, the diisocyanate is 35~45 parts by weight, polycaprolactone polyol or polytetramethylene ether diol
120~150 parts by weight, 0.1~1 parts by weight of dibutyl tin dilaurate, 10~20 parts by weight of dihydromethyl propionic acid and acetone 0.1
~1 parts by weight.
Preferably, the diisocyanate is toluene di-isocyanate(TDI), diphenyl methane -4,4,-two different hydrogen acid ether (hydrogen acid ester)s, different Buddhist
That at least one of the different hydrogen acid ether (hydrogen acid ester) of ketone two and hexamethylene diisocyanate.
Preferably, the relative molecular mass of the polycaprolactone polyol and polytetramethylene ether diol is 1000-2000；
The ratio (R value) of-OH is in-NCO and polycaprolactone polyol or polytetramethylene ether diol in isophorone diisocyanate
1.1~2.6；
Preferably ,-the NCO in the isophorone diisocyanate and the pure and mild polytetramethylene ether diol of polyester polyols
In-OH ratio (R value) be 1.4~2.2, studies have shown that R value on paper and aluminium foil combine performance characteristics have influence, this Shen
Please inventor by numerous studies find, in this preferred scope, binding performance is more preferably.
Preferably, the polyester polyol uses isocyanato silanes for the polyester polyol of initiator.
The present invention also provides the aqueous polyurethane emulsions in PET class compound adhesive, the transfer adhesive of paper and aluminium coated, multiple
Close the application of glue, Paper Coating.
The beneficial effects of the present invention are: the present invention saves production cost, together due to the reaction process of no added crosslinking agent
When solve the problems, such as that reaction is uneven, not easy to control, obtained aqueous polyurethane emulsion has preferable stability, glue film
With preferable mechanical property and folding resistance, adhesiveness, it is compound that aqueous polyurethane emulsion prepared by the present invention is applied to PET class
Transfer adhesive, compound adhesive, Paper Coating of glue, paper and aluminium coated etc., especially suitable for high-grade paper and aluminum transfer glue.Mainly
Product is improved to paper and aluminium foil high adhesion force and folding resistance.
Specific embodiment
Each raw material involved by following embodiment is the commercially available universal product unless otherwise instructed.
Embodiment 1
The embodiment of preparation method as aqueous polyurethane transfer adhesive of the invention, the preparation method include following
Step:
1) using the different hydrogen acid ether (hydrogen acid ester) of isophorone two, polycaprolactone polyol, polytetramethylene ether diol as raw material, tin dilaurate
Dibutyl tin is catalyst, adds dihydromethyl propionic acid, and acetone is added, and 85 degree of reactions obtain base polyurethane prepolymer for use as in 5 hours,
Middle R value is 1.4, and the relative molecular mass of polytetramethylene ether diol is 2000；
2) 60 degree are cooled to, triethanolamine neutralization reaction is added and generates salt, reacts 30min, wherein triethanolamine and dihydroxy
The molar ratio of methylpropanoic acid is 1:1, is down to room temperature, the aqueous solution that ethylenediamine is added is emulsified again chain extension 1 hour, ethylenediamine
Dosage is the 0.2% of prepolymer mass, and the dosage of water is 2 times of performed polymer gross mass；
3) finally, removing acetone under reduced pressure, aqueous polyurethane emulsion is obtained.
The aqueous polyurethane transfer adhesive of the present embodiment, the different hydrogen acid ether (hydrogen acid ester) of the isophorone two are 35 parts by weight, polycaprolactone
65 parts by weight of polyalcohol, 55 parts by weight of polytetramethylene ether diol, 0.1 parts by weight of dibutyl tin dilaurate, dihydroxymethyl third
0.1 parts by weight of sour 10 pbw acetone.
Embodiment 2
The embodiment of preparation method as aqueous polyurethane transfer adhesive of the invention, the preparation method include following
Step:
1) with toluene di-isocyanate(TDI), diphenyl methane -4,4,-two different hydrogen acid ether (hydrogen acid ester)s, polycaprolactone polyol are raw material, two
Dibutyl tin laurate is catalyst, adds dihydromethyl propionic acid, and proper amount of acetone is added, and 85 degree are reacted 5 hours, obtains poly- ammonia
Ester performed polymer, R value are 1.8, and the relative molecular mass of polycaprolactone polyol is 1000；
2) after being cooled to 60 degree, triethanolamine neutralization reaction is added and generates salt, reacts 30min, wherein triethanolamine and two
The molar ratio of hydroxymethyl propionic acid is 1:1, is down to room temperature, the aqueous solution that ethylenediamine is added is emulsified again chain extension 1 hour, ethylenediamine
Dosage be the 0.2% of prepolymer mass, the dosage of water is 2 times of performed polymer gross mass；
3) finally, removing acetone under reduced pressure, aqueous polyurethane emulsion is obtained.
The aqueous polyurethane transfer adhesive of the present embodiment, the toluene di-isocyanate(TDI) be 25 parts by weight, diphenyl methane -4,
4 ,-two different 10 parts by weight of hydrogen acid ether (hydrogen acid ester), 110 parts by weight of polycaprolactone polyol, 0.1 parts by weight of dibutyl tin dilaurate, dihydroxy
15 parts by weight of methylpropanoic acid, 0.1 parts by weight of acetone.
Embodiment 3
The embodiment of preparation method as aqueous polyurethane transfer adhesive of the invention, the preparation method include following
Step:
1) using hexamethylene diisocyanate, polycaprolactone polyol, polytetramethylene ether diol as raw material, tin dilaurate
Dibutyl tin is catalyst, adds dihydromethyl propionic acid, and proper amount of acetone is added, and 85 degree are reacted 5 hours, obtains polyurethane prepolymer
Body, wherein R value is 1.6, and the relative molecular mass of polycaprolactone polyol is 1000, the average molecular of polytetramethylene ether diol
Quality is 2000.
2) 60 degree are cooled to, triethanolamine neutralization reaction is added and generates salt, reacts 30min, triethanolamine and dihydroxymethyl
The molar ratio of propionic acid is 1:1, is down to room temperature, the aqueous solution that ethylenediamine is added is emulsified again chain extension 1 hour, the dosage of ethylenediamine
It is the 0.2% of prepolymer mass, the dosage of water is 2 times of performed polymer gross mass；
3) finally, removing acetone under reduced pressure, aqueous polyurethane emulsion is obtained.
The aqueous polyurethane transfer adhesive of the present embodiment, the hexamethylene diisocyanate are 40 parts by weight, polycaprolactone
75 parts by weight of polyalcohol, 65 parts by weight of polytetramethylene ether diol, 0.5 parts by weight of dibutyl tin dilaurate, dihydroxymethyl third
Sour 10 parts by weight, 0.5 parts by weight of acetone.
Embodiment 4
The embodiment of preparation method as aqueous polyurethane transfer adhesive of the invention, the preparation method include following
Step:
1) using the different hydrogen acid ether (hydrogen acid ester) of isophorone two, polycaprolactone polyol, polytetramethylene ether diol as raw material, tin dilaurate
Dibutyl tin is catalyst, adds dihydromethyl propionic acid, proper amount of acetone is added, and 85 degree are reacted 5 hours, and polyurethane prepolymer is obtained
Body, wherein R value is 1.1, and the relative molecular mass of polycaprolactone polyol is 1000；The average molecular of polytetramethylene ether diol
Quality is 2000；
2) 60 degree are cooled to, triethanolamine neutralization reaction is added and generates salt, reacts 30min, triethanolamine and dihydroxymethyl
The molar ratio of propionic acid is 1:1, is down to room temperature, the aqueous solution that ethylenediamine is added is emulsified again chain extension 1 hour, the dosage of ethylenediamine
It is the 0.2% of prepolymer mass, the dosage of water is 2 times of performed polymer gross mass；
3) finally, removing acetone under reduced pressure, aqueous polyurethane emulsion is obtained.
The aqueous polyurethane transfer adhesive of the present embodiment, the different hydrogen acid ether (hydrogen acid ester) of the isophorone two are 45 parts by weight, polycaprolactone
75 parts by weight of polyalcohol, 75 parts by weight of polytetramethylene ether diol, 1 parts by weight of dibutyl tin dilaurate, dihydromethyl propionic acid
15 parts by weight, 0.5 parts by weight of acetone.
Embodiment 5
The embodiment of preparation method as aqueous polyurethane transfer adhesive of the invention, the preparation method include following
Step:
1) using the different hydrogen acid ether (hydrogen acid ester) of isophorone two, polytetramethylene ether diol as raw material, dibutyl tin dilaurate is catalysis
Agent adds dihydromethyl propionic acid, and proper amount of acetone is added, and 85 degree are reacted 5 hours, obtains base polyurethane prepolymer for use as, wherein R value is
1.4, the relative molecular mass of polytetramethylene ether diol is 2000.
2) 60 degree are cooled to, triethanolamine neutralization reaction is added and generates salt, reacts 30min, triethanolamine and dihydroxymethyl
The molar ratio of propionic acid is 1:1, is down to room temperature, the aqueous solution that ethylenediamine is added is emulsified again chain extension 1 hour, the dosage of ethylenediamine
It is the 0.2% of prepolymer mass, the dosage of water is 2 times of performed polymer gross mass；
3) finally, removing acetone under reduced pressure, aqueous polyurethane emulsion is obtained.
The aqueous polyurethane transfer adhesive of the present embodiment, the different hydrogen acid ether (hydrogen acid ester) of the isophorone two are 45 parts by weight, poly- four methylene
150 parts by weight of base ether glycol, 1 parts by weight of dibutyl tin dilaurate, 20 parts by weight of dihydromethyl propionic acid, 1 parts by weight of acetone.
Embodiment 6
The embodiment of preparation method as aqueous polyurethane transfer adhesive of the invention, the preparation method include following
Step:
1) using the different hydrogen acid ether (hydrogen acid ester) of isophorone two, polycaprolactone polyol as raw material, dibutyl tin dilaurate is catalyst,
Dihydromethyl propionic acid is added, proper amount of acetone is added, 85 degree are reacted 5 hours, and base polyurethane prepolymer for use as is obtained, and wherein R value is 2.6,
The relative molecular mass of polycaprolactone polyol is 1000；
2) 60 degree are cooled to, triethanolamine neutralization reaction is added and generates salt, reacts 30min, triethanolamine and dihydroxymethyl
The molar ratio of propionic acid is 1:1, is down to room temperature, the aqueous solution that ethylenediamine is added is emulsified again chain extension 1 hour, the dosage of ethylenediamine
It is the 0.2% of prepolymer mass, the dosage of water is 2 times of performed polymer gross mass；
3) finally, removing acetone under reduced pressure, aqueous polyurethane emulsion is obtained.
Embodiment 7
The embodiment of preparation method as aqueous polyurethane transfer adhesive of the invention, the preparation method include following
Step:
1) using the different hydrogen acid ether (hydrogen acid ester) of isophorone two, polycaprolactone polyol, polytetramethylene ether diol as raw material, tin dilaurate
Dibutyl tin is catalyst, adds dihydromethyl propionic acid, and proper amount of acetone is added, and 85 degree are reacted 5 hours, obtains polyurethane prepolymer
Body, wherein R value is 2.2, and the relative molecular mass of polycaprolactone polyol is 1000, the average molecular of polytetramethylene ether diol
Quality is 2000.
2) 60 degree are cooled to, triethanolamine neutralization reaction is added and generates salt, reacts 30min, triethanolamine and dihydroxymethyl
The molar ratio of propionic acid is 1:1, is down to room temperature, the aqueous solution that ethylenediamine is added is emulsified again chain extension 1 hour, the dosage of ethylenediamine
It is the 0.2% of prepolymer mass, the dosage of water is 2 times of performed polymer gross mass.
3) finally, removing acetone under reduced pressure, aqueous polyurethane emulsion is obtained.
The aqueous polyurethane transfer adhesive of the present embodiment, the different hydrogen acid ether (hydrogen acid ester) of the isophorone two are 35 parts by weight, polycaprolactone
65 parts by weight of polyalcohol, 55 parts by weight of polytetramethylene ether diol, 0.1 parts by weight of dibutyl tin dilaurate, dihydroxymethyl third
0.1 parts by weight of sour 10 pbw acetone.
Embodiment 8
The embodiment of preparation method as aqueous polyurethane transfer adhesive of the invention, the preparation method include following
Step:
1) using the different hydrogen acid ether (hydrogen acid ester) of isophorone two, polycaprolactone polyol, polytetramethylene ether diol as raw material, tin dilaurate
Dibutyl tin is catalyst, adds dihydromethyl propionic acid, and proper amount of acetone is added, and 85 degree are reacted 5 hours, obtains polyurethane prepolymer
Body, R value are 2.6, and the relative molecular mass of polycaprolactone polyol is 1000, the relative molecular mass of polytetramethylene ether diol
It is 2000.
2) 60 degree are cooled to, triethanolamine neutralization reaction is added and generates salt, reacts 30min, triethanolamine and dihydroxymethyl
The molar ratio of propionic acid is 1:1, is down to room temperature, the aqueous solution that ethylenediamine is added is emulsified again chain extension 1 hour, the dosage of ethylenediamine
It is the 0.2% of prepolymer mass, the dosage of water is 2 times of performed polymer gross mass；
3) finally, removing acetone under reduced pressure, aqueous polyurethane emulsion is obtained.
The aqueous polyurethane transfer adhesive of the present embodiment, the different hydrogen acid ether (hydrogen acid ester) of the isophorone two are 35 parts by weight, polycaprolactone
65 parts by weight of polyalcohol, 55 parts by weight of polytetramethylene ether diol, 0.1 parts by weight of dibutyl tin dilaurate, dihydroxymethyl third
0.1 parts by weight of sour 10 pbw acetone.
Embodiment 9
The aqueous polyurethane emulsion characteristic that embodiment 1 to 8 is prepared is as shown in table 1 below:
Table 1
This implementation be also tested for by the aqueous polyurethane emulsion be used for transfer aluminum plated film, transfer laser film and art paper,
Hongta Huang core paper, Yi Gesende paper, Chinese paper and each germplasm bottom art post paperboard the compound bond properties of transfer, using of the invention
The method of aqueous polyurethane emulsion: 1) with before stirring evenly, the machine on suitable viscosity (not having to adjust under normal circumstances) that adjusts is applied
Cloth is coated on aluminum plated PET film surface；Dilutable water, to adjust suitably upper machine viscosity；2) gravure roll is once coated with, applicator roll
For 180-200/ inches of cable rolls；Three roller composite coatings, gluing composite roll hardness suggestion are 55~70 ° of dry-coated amount 1.5-
2.5g/m2；3) 200 mesh of circulation fluid are considered net filtration and are recycled, and foreign debris is avoided to influence coating composite effect；4) using heat
Wind or heat drying, it is 90-130m/min that 80-150 DEG C of drying temperature, which is suitable for speed,.
The test method of adhesion strength carries out test peel strength according to GB/T2791-1995.The results are shown in Table 2:
Table 2
As known from Table 1, lotion of the invention has stronger adhesion strength, best with the effect of embodiment 3.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (7)
1. a kind of preparation method of aqueous polyurethane emulsion, which comprises the following steps:
1) using diisocyanate, polycaprolactone polyol or/and polytetramethylene ether diol, dihydromethyl propionic acid as raw material, two
Dibutyl tin laurate is catalyst, and acetone is that reaction medium obtains base polyurethane prepolymer for use as；
2) triethylamine neutralization reaction is added and generates salt, the aqueous solution that ethylenediamine is added under high speed shear is emulsified chain extension again；
3) finally, removing acetone under reduced pressure, aqueous polyurethane emulsion is obtained.
2. the preparation method of aqueous polyurethane emulsion according to claim 1, which is characterized in that the diisocyanate is
120~150 parts by weight of 35~45 parts by weight, polycaprolactone polyol or polytetramethylene ether diol, dibutyl tin dilaurate
0.1~1 parts by weight of 0.1~1 parts by weight, 10~20 parts by weight of dihydromethyl propionic acid and acetone.
3. the preparation method of aqueous polyurethane emulsion according to claim 1, which is characterized in that the diisocyanate is
Toluene di-isocyanate(TDI), diphenyl methane -4,4, two isocyanide of-two different hydrogen acid ether (hydrogen acid ester)s, the different hydrogen acid ether (hydrogen acid ester) of isophorone two and hexa-methylene
At least one of acid esters.
4. the preparation method of aqueous polyurethane emulsion according to claim 1, which is characterized in that the polycaprolactone polyol
The relative molecular mass of pure and mild polytetramethylene ether diol is 1000~2000；- NCO in isophorone diisocyanate and poly-
The ratio of-OH is 1.1~2.6 in caprolactone polyol or polytetramethylene ether diol.
5. the preparation method of aqueous polyurethane emulsion according to claim 1, which is characterized in that the isophorone two is different
The ratio of-OH is 1.4~2.2 in the pure and mild polytetramethylene ether diol of-NCO and polyether polyols in cyanate.
6. the preparation method of aqueous polyurethane emulsion according to claim 1, which is characterized in that the polycaprolactone polyol
Alcohol uses isocyanato silanes for the polyester polyol of initiator.
7. a kind of if aqueous polyurethane emulsion as claimed in any one of claims 1 to 6 is in PET class compound adhesive, paper and aluminium coated
The application of transfer adhesive, compound adhesive, Paper Coating.
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| CN111269686A (en) * | 2020-04-03 | 2020-06-12 | 山东奥德美高分子材料有限公司 | High-fastness waterborne polyurethane transfer glue for offset printing |
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| CN115260443A (en) * | 2022-09-26 | 2022-11-01 | 石家庄鸿锐集团有限公司 | Waterborne polyurethane material and preparation method of waterborne polyurethane material applied to gloves |
| CN115449047A (en) * | 2022-07-07 | 2022-12-09 | 江西辙炜新材料科技有限公司 | Polyurethane latex, preparation method and application thereof |
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