CN106147383A - A kind of preparation method of the waterborne polyurethane resin for gravure compound oil ink - Google Patents
A kind of preparation method of the waterborne polyurethane resin for gravure compound oil ink Download PDFInfo
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- CN106147383A CN106147383A CN201610495707.3A CN201610495707A CN106147383A CN 106147383 A CN106147383 A CN 106147383A CN 201610495707 A CN201610495707 A CN 201610495707A CN 106147383 A CN106147383 A CN 106147383A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4244—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups
- C08G18/4247—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids
- C08G18/425—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids the polyols containing one or two ether groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6603—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6614—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6622—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3271
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- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses the preparation method of a kind of waterborne polyurethane resin for gravure compound oil ink, belong to ink material preparation field.This invention in turn includes the following steps: the synthesis of performed polymer, chain extending reaction prepares chain extending reaction thing, neutralize reaction and prepare amine salt type cation polyurethane neutralized reaction product, emulsion dispersion prepares amine salt type cation aqueous polyurethane, solvent distillation prepares content of acetone less than 0.1% amine salt type cation aqueous polyurethane, by amine salt type cation aqueous polyurethane is slowly added to wetting agent, levelling agent, thickening agent, adhesion promoter, coupling agent and deionized water during product configuration, prepare the waterborne polyurethane resin for gravure compound oil ink.Stable processing technique of the present invention, it is possible to meet for the adhesive force of multiple base material and combined strength bination in gravure compound oil ink prints, and do not fire, nontoxic and free from environmental pollution, meet the needs of environmental protection.
Description
Technical field
The invention belongs to ink material preparation field, be specifically related to the preparation method of a kind of waterborne polyurethane resin, specifically
Relate to a kind of water for gravure compound oil ink that the plastic sheeting for flexible package is had excellent adhesion and combined strength bination
The preparation method of property polyurethane resin.
Background technology
Along with environmental consciousness is gradually strengthened by the development of economic society, the increasingly stringent of environmental regulation and people, water
The research of property polyurethane increasingly comes into one's own.Aqueous polyurethane does not fire because it has, nontoxic, free from environmental pollution, the saving energy
And the easy advantage such as processing, according to formula and the different requirements of auxiliary agent, the adjustable process making coating, adhesive and other purposes
Agent.
Aqueous polyurethane be typically in pre-polymerization introduce hydrophilic chain extender, neutralized after, under high velocity agitation by ionizing
Polyurethane is added to the water, or adds water to polyurethane in aggressiveness organic solution, forms polyurethane aqueous dispersion.At present, to the moon
The research report of ion-type aqueous polyurethane is more, the most less to the research report of cation-type water-thinned polyurethane.Cation
Aqueous polyurethane all has preferable wettability, to part thereof such as polyethylene, polypropylene etc. to the material that hydrophobicity is stronger
Adhesive property is good, and has certain sterilization, dustproof effect, can be widely applied to be applied to the sides such as adhesive, coating, ink
Face.
At present, owing to the synthesis technique of cation aqueous polyurethane is not already sufficiently stable, with anion aqueous polyurethane
Comparing, due to the impact of reactivity, the synthesis of cation aqueous polyurethane is more difficult to realize, and industrialized production still has necessarily
Difficulty.Conventional its ionic dispersing group of cation aqueous polyurethane is generally quaternary or amine salt type, wherein with N-methyl
It is preferable that diethanolamine (N-MDEA) carries out emulsion dispersion effect as hydrophilic chain extender.Generally this type of cation aqueous polyurethane by
Pre-polymerization, chain extension introduce hydrophilic chain extender N methyldiethanol amine N-MDEA, and the most neutralized and emulsion dispersion step synthesizes, this work
In skill, volatile organic solvent (VOC) usage amount is more than more than 50%, as used some polyhydric alcohol VOC content even can be more than 75%
Above, this can not meet requirement prepared by current material greenization.
Summary of the invention
The technical problem to be solved is to overcome the above-mentioned deficiency in the presence of prior art, and provides a kind of raw
Production. art is stable, it is possible to meet in gravure compound oil ink prints for the adhesive force of multiple base material and combined strength bination needs
Preparation method for the waterborne polyurethane resin of gravure compound oil ink.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is: a kind of for gravure compound oil ink
The preparation method of waterborne polyurethane resin, it is characterised in that: the system of the described waterborne polyurethane resin for gravure compound oil ink
Preparation Method in turn includes the following steps:
(1) synthesis of performed polymer, described performed polymer comprises the raw material of following weight parts: polyhydric alcohol A10 part, polyhydric alcohol B2.0-50
Part, isocyanates 1.5-10 part, catalyst 0.01-0.03 part, acetone 3.0-12 part；By the polyhydric alcohol A of described weight portion with many
After unit alcohol B uniformly mixes, it is vacuum dried 1.0-2.0 hour under conditions of 100 DEG C-120 DEG C, is cooled to 60 DEG C-80 DEG C, by institute
Isocyanates and the catalyst of stating weight portion are slowly added in the mixture of polyhydric alcohol A and polyhydric alcohol B, 70 DEG C of-90 DEG C of conditions
Lower reaction 2.0-4.0 hour, measures isocyano (NCO) content and reaches stopped reaction during setting value, slow cooling to 60 DEG C,
The acetone of described weight portion is slowly added to, prepares described performed polymer；
(2) chain extending reaction, performed polymer addition step (1) prepared accounts for the hydrophilic chain extension that performed polymer mass percent is 4%-10%
The acetone soln of agent N methyldiethanol amine, reacts 2.0-4.0 hour under the conditions of 55 DEG C-65 DEG C, mensuration isocyano (
NCO) content reaches to add the acetone soln accounting for the polyhydric alcohol C that performed polymer mass percent is 0.5%-2% during setting value, slowly
Add and quickly stir, then reacting 1.0-2.0 hour under the conditions of 55 DEG C-65 DEG C, measuring isocyano (NCO) content and reach
Proceed reaction to adding isocyanate blocking agents during setting value, until reaction stops, preparing chain extending reaction thing；
(3) neutralizing reaction, the chain extending reaction thing that step (2) prepares is cooled to 50 DEG C, add glacial acetic acid and neutralize, regulation pH is extremely
6.0-8.0, addition accounts for chain extending reaction thing mass percent 35%-40% acetone and is diluted, quickly stirs under the conditions of 40 DEG C-50 DEG C
Mixing mixing 1.0 hours, make in the amido in chain extending reaction thing and become salt, degree of neutralization is 80%-100%, prepared amine salt type cation
Polyurethane neutralized reaction product；
(4) emulsion dispersion, under the conditions of temperature is 40 DEG C-50 DEG C, amine salt type cation polyurethane step (3) prepared neutralizes
Product at the uniform velocity adds by dropping mode the deionized water accounting for neutralized reaction product mass percent 65%-70%, and quickly stirs 10-20
Minute, then be slowly stirred 30 minutes, prepare amine salt type cation aqueous polyurethane；
(5) solvent distillation, utilizes vacuum decompression method to distill the amine salt type cation aqueous polyurethane that step (4) prepares,
Under conditions of vacuum 0.08MPa, temperature 50 C-60 DEG C, distill out acetone solvent, make amine salt type cation aqueous polyurethane
The content of middle acetone is less than 0.1%, prepares amine salt type cation aqueous polyurethane；
(6) product configuration, by step (5) prepare amine salt type cation aqueous polyurethane in be slowly added to wetting agent, levelling agent,
Thickening agent, adhesion promoter, coupling agent and deionized water, prepare the described aqueous polyurethane tree for gravure compound oil ink
Fat, every 100 parts of amine salt type cation aqueous polyurethane domestic demands add wetting agent 0.01-0.2 part, levelling agent 0.01-0.3 part, increasing
Thick dose of 0.1-0.5 part, adhesion promoter 0.1-1.0 part, coupling agent 0.1-1.0 part and deionized water 60-80 part.
Further, described polyhydric alcohol A is polyadipate-Isosorbide-5-Nitrae butanediol ester glycol, polyadipate-Isosorbide-5-Nitrae butanediol-second
Diol ester glycol, polyadipate-diethylene glycol esterdiol, polyadipate-terephthalic anhydride-binaryglycol ester binary, poly-neighbour
Phthalate anhydride-diethylene glycol esterdiol, polyadipate-ethylene glycol and 1,2-propylene glycol esterdiol, polyadipate-glycol ester glycol,
Polyadipate-1,6 hexanediol esterdiol, polyadipate-terephthalic anhydride-diethylene glycol esterdiol, polyadipate Oleum Ricini
One or more in esterdiol, PCDL.
Further, described polyhydric alcohol B is oxolane-propylene oxide copolymer glycols, polytetrahydrofuran diol, polyoxygenated
One or several in propylene glycol, Polyoxyethylene glycol, polypropylene oxide triol, polypropylene oxide-castor oil polyhydric alcohol etc.
Kind.
Further, during described catalyst is dibutyl tin laurate and triethylenediamine or tetrabutyl titanate
One of which.
Further, described polyhydric alcohol C is in ethylene glycol, diethylene glycol, BDO, glycerol, trimethylolpropane
One or more.
Further, the physical and chemical index of the described waterborne polyurethane resin for gravure compound oil ink is: solid content is
33%-37%, pH value is 6.0-8.0.
The present invention compared with prior art, has the following advantages that and effect: stable processing technique of the present invention is controlled, permissible
Realize industrialized production, meet economic benefit, and this invention is used for the waterborne polyurethane resin of gravure compound oil ink to hydrophobic
Property stronger material all there is preferable wettability, good to the adhesive property of part thereof such as polyethylene, polypropylene etc., and tool
There are certain sterilization, dustproof effect, can be widely applied to be applied to the aspects such as adhesive, coating, ink, applied widely, and
And during synthetic resin, volatile organic solvent (VOC) consumption is reduced about 25%, well below existing preparation work
In skill, volatile organic solvent (VOC) usage amount is more than more than 50%, even more than more than 75% technical specification, it is ensured that green, nothing
It is malicious and free from environmental pollution,
Disclosure satisfy that for the adhesive force of multiple base material and combined strength bination in gravure compound oil ink prints, and do not fire, nontoxic
With free from environmental pollution, meet the needs of environmental protection.
Detailed description of the invention
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment, and the present invention can be made further by described embodiment
Supplement and explanation, but the present invention is not limited to these embodiments.
Embodiment 1
A kind of preparation method for the waterborne polyurethane resin of gravure compound oil ink in turn includes the following steps:
(1) synthesis of performed polymer, takes the polyadipate-Isosorbide-5-Nitrae butanediol ester glycol of 10 parts and the oxolane-propylene oxide of 20 parts
After copolymer glycols uniformly mixes, it is vacuum dried 1.0-2.0 hour under conditions of 100 DEG C-120 DEG C, is cooled to 60 DEG C-80 DEG C,
The dibutyl tin laurate of the isocyanates of 3 parts and 0.01 part is slowly added to polyadipate-1,4 butanediol ester glycol and four
In the mixture of hydrogen furan-propylene oxide copolymer glycols, react 2.0-4.0 hour under the conditions of 70 DEG C-90 DEG C, measure Carbimide.
Root (NCO) content reaches stopped reaction during setting value 35%, and the acetone of 5 parts is slowly added to by slow cooling to 60 DEG C, prepares
Described performed polymer；
(2) chain extending reaction, performed polymer addition step (1) prepared accounts for the hydrophilic chain extension that performed polymer mass percent is 4%-10%
The acetone soln of agent N methyldiethanol amine, reacts 2.0-4.0 hour under the conditions of 55 DEG C-65 DEG C, mensuration isocyano (
NCO) content reaches to add the acetone soln accounting for the ethylene glycol that performed polymer mass percent is 0.5%-2% during setting value 55%, slow
Slow addition is also quickly stirred, and then reacts 1.0-2.0 hour under the conditions of 55 DEG C-65 DEG C, measures isocyano (NCO) content
Add isocyanate blocking agents when reaching 45% and proceed reaction, until reaction stops, preparing chain extending reaction thing；
(3) neutralizing reaction, the chain extending reaction thing that step (2) prepares is cooled to 50 DEG C, add glacial acetic acid and neutralize, regulation pH is extremely
6.0-8.0, addition accounts for chain extending reaction thing mass percent 35%-40% acetone and is diluted, quickly stirs under the conditions of 40 DEG C-50 DEG C
Mixing mixing 1.0 hours, make in the amido in chain extending reaction thing and become salt, degree of neutralization is 80%-100%, prepared amine salt type cation
Polyurethane neutralized reaction product；
(4) emulsion dispersion, under the conditions of temperature is 40 DEG C-50 DEG C, amine salt type cation polyurethane step (3) prepared neutralizes
Product at the uniform velocity adds by dropping mode the deionized water accounting for neutralized reaction product mass percent 65%-70%, and quickly stirs 10-20
Minute, then be slowly stirred 30 minutes, prepare amine salt type cation aqueous polyurethane；
(5) solvent distillation, utilizes vacuum decompression method to distill the amine salt type cation aqueous polyurethane that step (4) prepares,
Under conditions of vacuum 0.08MPa, temperature 50 C-60 DEG C, distill out acetone solvent, make amine salt type cation aqueous polyurethane
The content of middle acetone is less than 0.1%, prepares amine salt type cation aqueous polyurethane；
(6) product configuration, by step (5) prepare amine salt type cation aqueous polyurethane in be slowly added to wetting agent, levelling agent,
Thickening agent, adhesion promoter, coupling agent and deionized water, prepare the described aqueous polyurethane tree for gravure compound oil ink
Fat.Wherein, every 100 parts of amine salt type cation aqueous polyurethane domestic demands add wetting agent 0.1 part, levelling agent 0.2 part, thickening agent
0.3 part, adhesion promoter 0.5 part, coupling agent 0.5 part and deionized water 70 parts.
Embodiment 2
A kind of preparation method for the waterborne polyurethane resin of gravure compound oil ink in turn includes the following steps:
(1) synthesis of performed polymer, takes the poly-phthalic anhydride-diethylene glycol esterdiol of 10 parts and the PolyTHF two of 20 parts
After alcohol uniformly mixes, it is vacuum dried 1.0-2.0 hour under conditions of 100 DEG C-120 DEG C, is cooled to 60 DEG C-80 DEG C, by 3 parts
Isocyanates and the triethylenediamine of 0.01 part or tetrabutyl titanate are slowly added to poly-phthalic anhydride-binaryglycol ester
In the mixture of glycol and polytetrahydrofuran diol, react 2.0-4.0 hour under the conditions of 70 DEG C-90 DEG C, measure isocyano
(NCO) content reaches stopped reaction during setting value 40%, slow cooling to 60 DEG C, is slowly added to by the acetone of 5 parts, prepares institute
State performed polymer；
(2) chain extending reaction, performed polymer addition step (1) prepared accounts for the hydrophilic chain extension that performed polymer mass percent is 4%-10%
The acetone soln of agent N methyldiethanol amine, reacts 2.0-4.0 hour under the conditions of 55 DEG C-65 DEG C, mensuration isocyano (
NCO) content reaches to add during setting value 50% that to account for the acetone of the 1,4-butanediol that performed polymer mass percent is 0.5%-2% molten
Liquid, is slowly added to and quickly stirs, and then reacts 1.0-2.0 hour under the conditions of 55 DEG C-65 DEG C, mensuration isocyano (
NCO) when content reaches 35%, addition isocyanate blocking agents proceeds reaction, until reaction stops, preparing chain extending reaction thing；
(3) neutralizing reaction, the chain extending reaction thing that step (2) prepares is cooled to 50 DEG C, add glacial acetic acid and neutralize, regulation pH is extremely
6.0-8.0, addition accounts for chain extending reaction thing mass percent 35%-40% acetone and is diluted, quickly stirs under the conditions of 40 DEG C-50 DEG C
Mixing mixing 1.0 hours, make in the amido in chain extending reaction thing and become salt, degree of neutralization is 80%-100%, prepared amine salt type cation
Polyurethane neutralized reaction product；
(4) emulsion dispersion, under the conditions of temperature is 40 DEG C-50 DEG C, amine salt type cation polyurethane step (3) prepared neutralizes
Product at the uniform velocity adds by dropping mode the deionized water accounting for neutralized reaction product mass percent 65%-70%, and quickly stirs 10-20
Minute, then be slowly stirred 30 minutes, prepare amine salt type cation aqueous polyurethane；
(5) solvent distillation, utilizes vacuum decompression method to distill the amine salt type cation aqueous polyurethane that step (4) prepares,
Under conditions of vacuum 0.08MPa, temperature 50 C-60 DEG C, distill out acetone solvent, make amine salt type cation aqueous polyurethane
The content of middle acetone is less than 0.1%, prepares amine salt type cation aqueous polyurethane；
(6) product configuration, by step (5) prepare amine salt type cation aqueous polyurethane in be slowly added to wetting agent, levelling agent,
Thickening agent, adhesion promoter, coupling agent and deionized water, prepare the described aqueous polyurethane tree for gravure compound oil ink
Fat.Wherein, every 100 parts of amine salt type cation aqueous polyurethane domestic demands add wetting agent 0.15 part, levelling agent 0.25 part, thickening agent
0.4 part, adhesion promoter 0.8 part, coupling agent 0.7 part and deionized water 75 parts.
Although the present invention is open as above with embodiment, but it is not limited to protection scope of the present invention, any ripe
Know the technical staff of this technology, in the change made without departing from the spirit and scope of the invention and retouching, all should be belonged to this
The protection domain of invention.
Claims (6)
1. the preparation method for the waterborne polyurethane resin of gravure compound oil ink, it is characterised in that: described for gravure
The preparation method of the waterborne polyurethane resin of compound oil ink in turn includes the following steps:
(1) synthesis of performed polymer, described performed polymer comprises the raw material of following weight parts: polyhydric alcohol A10 part, polyhydric alcohol B2.0-50
Part, isocyanates 1.5-10 part, catalyst 0.01-0.03 part, acetone 3.0-12 part；By the polyhydric alcohol A of described weight portion with many
After unit alcohol B uniformly mixes, it is vacuum dried 1.0-2.0 hour under conditions of 100 DEG C-120 DEG C, is cooled to 60 DEG C-80 DEG C, by institute
Isocyanates and the catalyst of stating weight portion are slowly added in the mixture of polyhydric alcohol A and polyhydric alcohol B, 70 DEG C of-90 DEG C of conditions
Lower reaction 2.0-4.0 hour, measures isocyano (NCO) content and reaches stopped reaction during setting value, slow cooling to 60 DEG C,
The acetone of described weight portion is slowly added to, prepares described performed polymer；
(2) chain extending reaction, performed polymer addition step (1) prepared accounts for the hydrophilic chain extension that performed polymer mass percent is 4%-10%
The acetone soln of agent N methyldiethanol amine, reacts 2.0-4.0 hour under the conditions of 55 DEG C-65 DEG C, mensuration isocyano (
NCO) content reaches to add the acetone soln accounting for the polyhydric alcohol C that performed polymer mass percent is 0.5%-2% during setting value, slowly
Add and quickly stir, then reacting 1.0-2.0 hour under the conditions of 55 DEG C-65 DEG C, measuring isocyano (NCO) content and reach
Proceed reaction to adding isocyanate blocking agents during setting value, until reaction stops, preparing chain extending reaction thing；
(3) neutralizing reaction, the chain extending reaction thing that step (2) prepares is cooled to 50 DEG C, add glacial acetic acid and neutralize, regulation pH is extremely
6.0-8.0, addition accounts for chain extending reaction thing mass percent 35%-40% acetone and is diluted, quickly stirs under the conditions of 40 DEG C-50 DEG C
Mixing mixing 1.0 hours, make in the amido in chain extending reaction thing and become salt, degree of neutralization is 80%-100%, prepared amine salt type cation
Polyurethane neutralized reaction product；
(4) emulsion dispersion, under the conditions of temperature is 40 DEG C-50 DEG C, amine salt type cation polyurethane step (3) prepared neutralizes
Product at the uniform velocity adds by dropping mode the deionized water accounting for neutralized reaction product mass percent 65%-70%, and quickly stirs 10-20
Minute, then be slowly stirred 30 minutes, prepare amine salt type cation aqueous polyurethane；
(5) solvent distillation, utilizes vacuum decompression method to distill the amine salt type cation aqueous polyurethane that step (4) prepares,
Under conditions of vacuum 0.08MPa, temperature 50 C-60 DEG C, distill out acetone solvent, make amine salt type cation aqueous polyurethane
The content of middle acetone is less than 0.1%, prepares amine salt type cation aqueous polyurethane；
(6) product configuration, by step (5) prepare amine salt type cation aqueous polyurethane in be slowly added to wetting agent, levelling agent,
Thickening agent, adhesion promoter, coupling agent and deionized water, prepare the described aqueous polyurethane tree for gravure compound oil ink
Fat, every 100 parts of amine salt type cation aqueous polyurethane domestic demands add wetting agent 0.01-0.2 part, levelling agent 0.01-0.3 part, increasing
Thick dose of 0.1-0.5 part, adhesion promoter 0.1-1.0 part, coupling agent 0.1-1.0 part and deionized water 60-80 part.
The preparation method of a kind of waterborne polyurethane resin for gravure compound oil ink the most according to claim 1, it is special
Levy and be: described polyhydric alcohol A be polyadipate-1,4 butanediol ester glycol, polyadipate-1,4 butanediols-glycol ester glycol,
Polyadipate-diethylene glycol esterdiol, polyadipate-terephthalic anhydride-binaryglycol ester binary, poly-phthalic anhydride-
Diethylene glycol esterdiol, polyadipate-ethylene glycol and 1,2-propylene glycol esterdiol, polyadipate-glycol ester glycol, polyadipate-1,
6 hexanediol esterdiols, polyadipate-terephthalic anhydride-diethylene glycol esterdiol, polyadipate Oleum Ricini esterdiol, poly-carbon
One or more in acid esters glycol.
The preparation method of a kind of waterborne polyurethane resin for gravure compound oil ink the most according to claim 1, it is special
Levy and be: described polyhydric alcohol B be oxolane-propylene oxide copolymer glycols, polytetrahydrofuran diol, polyoxypropyleneglycol,
One or more in Polyoxyethylene glycol, polypropylene oxide triol, polypropylene oxide-castor oil polyhydric alcohol etc..
The preparation method of a kind of waterborne polyurethane resin for gravure compound oil ink the most according to claim 1, it is special
Levy and be: described catalyst is the one of which in dibutyl tin laurate and triethylenediamine or tetrabutyl titanate.
The preparation method of a kind of waterborne polyurethane resin for gravure compound oil ink the most according to claim 1, it is special
Levy and be: described polyhydric alcohol C is one or more in ethylene glycol, diethylene glycol, 1,4-butanediol, glycerol, trimethylolpropane.
The preparation method of a kind of waterborne polyurethane resin for gravure compound oil ink the most according to claim 1, it is special
Levy and be: the physical and chemical index of the described waterborne polyurethane resin for gravure compound oil ink is: solid content is 33%-37%, pH value
For 6.0-8.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610495707.3A CN106147383A (en) | 2016-06-30 | 2016-06-30 | A kind of preparation method of the waterborne polyurethane resin for gravure compound oil ink |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610495707.3A CN106147383A (en) | 2016-06-30 | 2016-06-30 | A kind of preparation method of the waterborne polyurethane resin for gravure compound oil ink |
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| CN109485815A (en) * | 2018-10-15 | 2019-03-19 | 中山大学 | A kind of preparation method of aqueous polyurethane emulsion and its aqueous polyurethane emulsion obtained and its application |
| CN109485815B (en) * | 2018-10-15 | 2021-01-01 | 中山大学 | Preparation method of waterborne polyurethane emulsion, waterborne polyurethane emulsion prepared by preparation method and application of waterborne polyurethane emulsion |
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