CN110938330B - Water-based ink and preparation method thereof - Google Patents

Water-based ink and preparation method thereof Download PDF

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CN110938330B
CN110938330B CN201911274361.4A CN201911274361A CN110938330B CN 110938330 B CN110938330 B CN 110938330B CN 201911274361 A CN201911274361 A CN 201911274361A CN 110938330 B CN110938330 B CN 110938330B
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parts
polyurethane emulsion
water
ink
aqueous
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CN110938330A (en
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包亚群
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Guangzhou 1s Environmental Protection Technology Co ltd
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Guangzhou 1s Environmental Protection Technology Co ltd
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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
    • 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
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • 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
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
    • 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
    • C09D11/104—Polyesters

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)

Abstract

The invention provides water-based ink and a preparation method and application thereof, wherein the water-based ink comprises the following components: the paint comprises aqueous polyurethane emulsion, a dispersant, pigment and water; the aqueous polyurethane emulsion comprises aliphatic polycarbonate type aqueous polyurethane emulsion and aliphatic polyester type aqueous polyurethane emulsion. The water-based ink disclosed by the invention is compounded by adopting the two water-based polyurethane emulsions, so that the formed ink layer has the characteristics of high hardness, strong adhesive force, high glossiness and good flexibility of the aliphatic polyester water-based polyurethane after the aliphatic polycarbonate water-based polyurethane is formed into a film, and the prepared ink has proper viscosity and good dispersion stability by matching with a dispersing agent, a pigment and water.

Description

Water-based ink and preparation method thereof
Technical Field
The invention relates to the field of fine chemical engineering, and particularly relates to water-based ink and a preparation method thereof.
Background
With the rapid development of economy in China and the improvement of living standard of people, the environmental protection health consciousness of people is gradually improved, and the environment protection strategy of sustainable development is also put forward by the nation. With the improvement of national environmental laws and regulations and the enhancement of environmental awareness of people, the traditional solvent-based screen printing ink is more and more limited in use because the emission of VOC (volatile organic gas) in the ink harms the health of operators and causes serious pollution to the environment. China printing enters the environment-friendly era, and is new and expensive as environment-friendly ink, and the research and application of water-based ink are more and more paid attention by people.
CN103980461 discloses a method for preparing a hydrolysis-resistant aqueous polyurethane dispersion, which comprises synthesizing a polyurethane prepolymer for crosslinking modification, adding an end-capping agent 1-aminopropyl-2-methylimidazole for end-capping emulsification, and obtaining the aqueous polyurethane with good water resistance.
CN103910851 discloses a preparation method of a waterborne polyurethane binder, the binder prepared by the method has good adhesion fastness to plastic films, good water resistance and boiling resistance, and excellent comprehensive performance, but the method is used for feeding materials in batches for many times, and the technological process is complex.
Therefore, there is a strong demand in the market to develop a water-based ink which is easy and safe to use and has excellent comprehensive properties.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a water-based ink and a preparation method and application thereof. The water-based ink disclosed by the invention is prepared by compounding the aliphatic polycarbonate water-based polyurethane emulsion and the aliphatic polyester water-based polyurethane emulsion, so that the prepared ink layer has high adhesive force and high chemical resistance, and then the dispersing agent, the pigment and the water are matched, so that the prepared ink has proper viscosity and good dispersion stability.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides an aqueous ink comprising the following components: the paint comprises aqueous polyurethane emulsion, a dispersant, pigment and water; the aqueous polyurethane emulsion comprises aliphatic polycarbonate type aqueous polyurethane emulsion and aliphatic polyester type aqueous polyurethane emulsion.
According to the invention, the water-based ink is specifically compounded by adopting the aliphatic polycarbonate water-based polyurethane emulsion and the aliphatic polyester water-based polyurethane emulsion, so that the formed ink layer has the characteristics of high hardness, strong adhesive force, high glossiness and good flexibility of the aliphatic polyester water-based polyurethane after the aliphatic polycarbonate water-based polyurethane is formed into a film, and then the prepared ink has proper viscosity and good dispersion stability by matching with the dispersant, the pigment and water.
According to the water-based ink, the aliphatic polycarbonate water-based polyurethane emulsion and the aliphatic polyester water-based polyurethane emulsion are controlled at a certain temperature under the action of the isocyanate curing agent, so that cross-linking and curing can be realized, wherein the two water-based polyurethane emulsions can be matched with each other to realize synergistic interaction, the defect of single use of the two emulsions is effectively overcome, and the prepared water-based ink layer has good hardness, adhesive force and flexibility.
Preferably, the water-based ink comprises the following components in parts by weight: 20-70 parts of waterborne polyurethane emulsion, 0.1-2 parts of dispersant, 5-20 parts of pigment and 10-30 parts of water.
The amount of the aqueous polyurethane emulsion is, for example, 20 to 70 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, or the like.
The dispersant may be used in an amount of 0.1 to 2 parts, for example, 0.1 part, 0.3 part, 0.5 part, 0.8 part, 1 part, 1.3 parts, 1.5 parts, 1.8 parts, or 2 parts.
The pigment is 5 to 20 parts, for example, 5 parts, 8 parts, 10 parts, 12 parts, 15 parts, 18 parts, or 20 parts.
The amount of water is 10 to 30 parts, and may be, for example, 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, 22 parts, 25 parts, 27 parts, 29 parts, 30 parts, or the like.
Preferably, the water-based ink comprises the following components in parts by weight: 20-50 parts of waterborne polyurethane emulsion, 0.1-2 parts of dispersant, 5-15 parts of pigment and 10-30 parts of water.
The mass ratio of the aliphatic polycarbonate aqueous polyurethane emulsion to the aliphatic polyester aqueous polyurethane emulsion is preferably (0.5 to 2: 1), and may be, for example, 0.5:1, 0.6:1, 0.7:1, 0.8:1, 0.9:1, 1:1, 1.1:1, 1.2:1, 1.3:1, 1.4:1, 1.5:1, 1.6:1, 1.7:1, 1.8:1, 1.9:1 or 2:1, and preferably 1: 1.
The invention preferably controls the mass ratio of the two waterborne polyurethane emulsions, and mainly aims to ensure the comprehensive improvement of the comprehensive performance of the prepared ink layer. When the mass ratio of the aliphatic polycarbonate type aqueous polyurethane emulsion to the aliphatic polycarbonate type aqueous polyurethane emulsion is higher than the above range, the hard segment structure in the molecular structure of the prepared ink layer is more, and the ink layer is crisp in texture and poor in flexibility after being cured into a film; when the mass ratio of the aliphatic polyester type aqueous polyurethane emulsion to the aliphatic polyester type aqueous polyurethane emulsion is lower than the range, the content of the aliphatic polyester type aqueous polyurethane emulsion is higher, so that the number of soft segment structures in the molecular structure of the prepared ink layer is larger, the surface of a cured film-forming thick film is easy to be sticky, the hardness is low, the adhesion force is poor, and the construction performance is obviously poor.
Preferably, the aliphatic polycarbonate-type aqueous polyurethane emulsion has a solid content of 25 to 35%, and for example, may be 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%, or the like.
The viscosity of the aliphatic polycarbonate-based aqueous polyurethane emulsion is preferably less than 250 mPas, and may be, for example, 250 mPas, 230 mPas, 200 mPas, 180 mPas, 150 mPas, 120 mPas, 100 mPas, 80 mPas or 50 mPas.
Preferably, the aliphatic polycarbonate-type aqueous polyurethane emulsion has a pH of 8.5 to 9.5, and may be, for example, 8.5, 8.6, 8.8, 9.0, 9.2, 9.3, 9.4, 9.5, or the like.
Preferably, the tensile strength of the polyurethane in the aliphatic polycarbonate type aqueous polyurethane emulsion after film formation is 15-20N/mm2For example, it may be 15N/mm2、16N/mm2、17N/mm2、18N/mm2、19N/mm2Or 20N/mm2And the like.
Preferably, the elongation at break after film formation of the polyurethane in the aliphatic polycarbonate-based aqueous polyurethane emulsion is 300% to 500%, and may be, for example, 300%, 350%, 400%, 450%, or 500%.
Preferably, the solid content of the aliphatic polyester-based aqueous polyurethane emulsion is 30 to 40%, and may be, for example, 30%, 32%, 33%, 35%, 36%, 38%, 39%, 40%, or the like.
The viscosity of the aliphatic polyester-based aqueous polyurethane emulsion is preferably less than 500 mPas, and may be, for example, 500 mPas, 450 mPas, 400 mPas, 350 mPas, 300 mPas, 250 mPas, 200 mPas, 250 mPas or 100 mPas.
Preferably, the pH of the aliphatic polyester-based aqueous polyurethane emulsion is 8.5 to 9.5, and may be, for example, 8.5, 8.6, 8.8, 9.0, 9.2, 9.3, 9.4, 9.5, or the like.
Preferably, the tensile strength of the aliphatic polyester type waterborne polyurethane emulsion after the polyurethane film forming is 15-20N/mm2For example, it may be 15N/mm2、16N/mm2、17N/mm2、18N/mm2、19N/mm2Or 20N/mm2And the like.
Preferably, the elongation at break after film formation of polyurethane in the aliphatic polyester-based aqueous polyurethane emulsion is 500% to 700%, and may be, for example, 500%, 550%, 600%, 650%, or 700%.
Preferably, the dispersant is Solsperse 27000.
Preferably, the pigment is selected from any one or a combination of at least two of carbon black, titanium dioxide, aniline yellow, phthalocyanine blue or ultramarine blue.
Preferably, the aqueous ink further comprises 10-40 parts of a filler, which may be, for example, 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, or the like.
Preferably, the filler comprises any one of barium sulfate, talc or alumina powder or a combination of at least two thereof.
Preferably, the aqueous ink further comprises 1-5 parts of an auxiliary agent, which may be 1 part, 2 parts, 3 parts, 4 parts, 5 parts, or the like.
Preferably, the assistant comprises 0.1-0.5 parts of leveling agent, for example, 0.1 part, 0.2 part, 0.3 part, 0.4 part or 0.5 part, etc.
Preferably, the leveling agent is an acrylate leveling agent, preferably BYK-3560 and/or BYK-3565.
Preferably, the adjuvant further comprises 0.1 to 1 part of a pH stabilizer, which may be, for example, 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, or 1 part.
Preferably, the pH stabilizer is AMP-95.
Preferably, the adjuvant further comprises 0.1-0.5 parts of bactericide, which can be 0.1 part, 0.2 part, 0.3 part, 0.4 part or 0.5 part, etc.
Preferably, the bactericide is KATHON LXE.
Preferably, the adjuvant further comprises 1-3 parts of a defoamer, which may be, for example, 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts, or the like.
Preferably, the defoaming agent is a non-silicone defoaming agent, preferably BYK-015 and/or BYK-1710.
In a second aspect, the present invention also provides a method for preparing the aqueous ink according to the first aspect, the method comprising: mixing the aqueous polyurethane emulsion, a dispersant, a pigment, water, optional fillers and optional auxiliaries to obtain the aqueous ink.
The preparation method of the water-based ink only needs to simply mix the preparation raw materials, is simple and easy to operate, and has wide application prospect.
Preferably, the mixing method is as follows: the aqueous polyurethane emulsion, the dispersant, the pigment, water and optionally the pigment are premixed, and then the optionally auxiliary agent is added into the premixed system for remixing.
Preferably, the temperature of the pre-mixing is 40-60 ℃, for example, 40 ℃, 45 ℃, 50 ℃, 55 ℃ or 60 ℃ and the like.
Preferably, the time for the premixing is 30min or more, for example, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min, 150min, or 200min, and preferably 60 to 120 min.
Preferably, the stirring speed of the premixing is 300-.
Preferably, the system after premixing is ground to a fineness of <5 μm, which may be, for example, 5 μm, 4.5 μm, 4 μm, 3.5 μm, 3 μm, 2.5 μm or 2 μm, etc., before the optional auxiliaries are added.
Preferably, the pre-mixed system is cooled to 18-30 ℃ before adding the optional auxiliary agents, which may be 18 ℃, 20 ℃, 22 ℃, 25 ℃, 28 ℃ or 30 ℃ for example.
In a third aspect, the present invention also provides an ink layer obtained by curing the water-based ink according to the first aspect and a curing agent.
Preferably, the curing agent is an isocyanate curing agent.
Preferably, the isocyanate curing agent is added in an amount of 1 to 5 wt%, for example, 1 wt%, 2 wt%, 3 wt%, 4 wt%, or 5 wt% based on the total mass of the aliphatic polycarbonate-based aqueous polyurethane emulsion and the aliphatic polyester-based aqueous polyurethane emulsion.
According to the ink layer, the isocyanate curing agent is added into the water-based ink, and hydroxyl groups on polyurethane molecular chains contained in the aliphatic polycarbonate type water-based polyurethane emulsion and the aliphatic polyester type water-based polyurethane emulsion can react with isocyanate groups on the isocyanate molecular chains, namely, the two polyurethane molecular chains are crosslinked through the isocyanate curing agent, so that the two polyurethanes can be mutually matched, the synergy is realized, and various performances of the ink layer are comprehensively improved.
In a fourth aspect, the present invention also provides a method for preparing the ink layer according to the third aspect, wherein the method for preparing the ink layer comprises: and mixing the water-based ink and a curing agent, printing a first layer on the surface of the base material by using the obtained mixture, drying the surface, then printing a second layer, drying the surface, repeating the printing and drying process, printing an Nth layer, drying the surface and curing to obtain the ink layer.
In the present invention, N in the Nth layer means 3 or more.
Preferably, the temperature of the surface drying is 70-100 ℃, for example, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃ or 100 ℃ and the like.
Preferably, the surface drying time is 3-20min, such as 3min, 5min, 8min, 10min, 12min, 15min, 17min or 20 min.
Preferably, the curing temperature is 70-100 ℃, for example, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃ or 100 ℃.
Preferably, the curing time is 60-120min, for example, 60min, 70min, 80min, 90min, 100min, 110min or 120min, etc.
Preferably, the preparation method comprises: mixing water-based ink and a curing agent, firstly printing a first layer on the surface of a base material, performing surface drying at 70-100 ℃ for 3-20min, then printing a second layer, performing surface drying at 70-100 ℃ for 3-20min, repeating the printing and surface drying process, printing an Nth layer, performing surface drying at 70-100 ℃ for 3-20min, and then curing at 70-100 ℃ for 60-120min to obtain the ink layer.
In a fourth aspect, the present invention also provides a use of the aqueous ink according to the first aspect in a Polycarbonate (PC) ink, a polyethylene terephthalate (PET) ink or a composite ink.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the water-based ink, the aliphatic polycarbonate type water-based polyurethane emulsion and the aliphatic polyester type water-based polyurethane emulsion are compounded, so that the formed ink layer has the characteristics of high hardness, strong adhesive force, high glossiness and good flexibility of the aliphatic polyester type water-based polyurethane after the aliphatic polycarbonate type water-based polyurethane is formed into a film, and the prepared ink has proper viscosity and good dispersion stability by matching with the dispersing agent, the pigment and the water;
(2) according to the water-based ink, under the action of an isocyanate curing agent, the aliphatic polycarbonate water-based polyurethane emulsion and the aliphatic polyester water-based polyurethane emulsion are controlled at a certain temperature, so that crosslinking and curing can be realized, wherein the two water-based polyurethane emulsions can be matched with each other to realize synergistic interaction, so that the defect of single use of the two emulsions is effectively overcome, and the prepared water-based ink layer has good hardness, adhesive force and flexibility;
(3) the water-based ink disclosed by the invention takes water as a dispersing agent, is environment-friendly and harmless to a human body, and also has the advantages of difficulty in combustion, easiness in obtaining raw materials, low cost and the like.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The manufacturers and the brands of the aliphatic polycarbonate type aqueous polyurethane emulsion and the aliphatic polyester type aqueous polyurethane emulsion used in the examples and the comparative examples of the present invention are as follows:
aliphatic polycarbonate type aqueous polyurethane emulsion (available from Shanghai Jinhui chemical Co., Ltd., trademark: Relca PU-477);
aliphatic polyester type aqueous polyurethane emulsion (available from Shanghai Jinghui chemical Co., Ltd., under the trademark Picassian PU-968).
Example 1
The embodiment provides a water-based ink and a preparation method thereof.
The water-based ink comprises the following components in parts by weight: 30 parts of aliphatic polycarbonate type aqueous polyurethane emulsion, 30 parts of aliphatic polyester type aqueous polyurethane emulsion, 1 part of Solsperse 27000 dispersant, 10 parts of carbon black, 20 parts of barium sulfate, 10 parts of talcum powder, 0.5 part of BYK-3565 flatting agent, 0.5 part of AMP-95pH stabilizer, 0.1 part of KATHON LXE bactericide, 1.5 parts of BYK-015 defoaming agent and 20 parts of water, wherein the mass ratio of the aliphatic polycarbonate type aqueous polyurethane emulsion to the aliphatic polyester type aqueous polyurethane emulsion is 1: 1.
The preparation method comprises the following steps:
firstly premixing an aliphatic polycarbonate type waterborne polyurethane emulsion, an aliphatic polyester type waterborne polyurethane emulsion, a Solsperse 27000 dispersant, carbon black, barium sulfate, talcum powder and water at 55 ℃ for 70min at a stirring speed of 500rpm, grinding to the fineness of 3 mu m, cooling to 20 ℃, adding the rest components into the premixed system, and then mixing to obtain the water-based ink.
Example 2
The embodiment provides a water-based ink and a preparation method thereof.
The water-based ink comprises the following components in parts by weight: 40 parts of aliphatic polycarbonate type aqueous polyurethane emulsion, 30 parts of aliphatic polyester type aqueous polyurethane emulsion, 2 parts of Solsperse 27000 dispersant, 5 parts of carbon black, 15 parts of barium sulfate, 10 parts of talcum powder, 0.1 part of BYK-3565 flatting agent, 0.1 part of AMP-95pH stabilizer, 0.4 part of KATHON LXE bactericide, 1 part of BYK-015 defoaming agent and 20 parts of water, wherein the mass ratio of the aliphatic polycarbonate type aqueous polyurethane emulsion to the aliphatic polyester type aqueous polyurethane emulsion is 1.33: 1.
The preparation method comprises the following steps:
the water-based ink is prepared by premixing aliphatic polycarbonate type water-based polyurethane emulsion, aliphatic polyester type water-based polyurethane emulsion, Solsperse 27000 dispersant, carbon black, barium sulfate, talcum powder and water at 60 ℃ and at a stirring speed of 700rpm for 80min, grinding to the fineness of 4 mu m, cooling to 30 ℃, adding the rest components into the premixed system, and then mixing to obtain the water-based ink.
Example 3
The embodiment provides a water-based ink and a preparation method thereof.
The water-based ink comprises the following components in parts by weight: 20 parts of aliphatic polycarbonate type aqueous polyurethane emulsion, 40 parts of aliphatic polyester type aqueous polyurethane emulsion, 2 parts of Solsperse 27000 dispersant, 20 parts of ultramarine blue, 10 parts of barium sulfate, 5 parts of talcum powder, 0.2 part of BYK-3565 flatting agent, 1 part of AMP-95pH stabilizer, 0.4 part of KATHON LXE bactericide, 3 parts of BYK-015 defoaming agent and 22 parts of water, wherein the mass ratio of the aliphatic polycarbonate type aqueous polyurethane emulsion to the aliphatic polyester type aqueous polyurethane emulsion is 0.5: 1.
The preparation method comprises the following steps:
firstly premixing an aliphatic polycarbonate type waterborne polyurethane emulsion, an aliphatic polyester type waterborne polyurethane emulsion, a Solsperse 27000 dispersant, ultramarine blue, barium sulfate, talcum powder and water at 40 ℃ at a stirring speed of 1000rpm for 120min, grinding to the fineness of 3 mu m, cooling to 23 ℃, adding the rest components into the premixed system, and then mixing to obtain the waterborne ink.
Example 4
The embodiment provides a water-based ink and a preparation method thereof.
The water-based ink comprises the following components in parts by weight: 40 parts of aliphatic polycarbonate type aqueous polyurethane emulsion, 20 parts of aliphatic polyester type aqueous polyurethane emulsion, 2 parts of Solsperse 27000 dispersant, 10 parts of phthalocyanine blue, 10 parts of barium sulfate, 10 parts of talcum powder, 0.1 part of BYK-3565 flatting agent, 1 part of AMP-95pH stabilizer, 0.5 part of KATHON LXE bactericide, 2 parts of BYK-015 defoaming agent and 28 parts of water, wherein the mass ratio of the aliphatic polycarbonate type aqueous polyurethane emulsion to the aliphatic polyester type aqueous polyurethane emulsion is 2: 1.
The preparation method comprises the following steps:
firstly premixing an aliphatic polycarbonate type waterborne polyurethane emulsion, an aliphatic polyester type waterborne polyurethane emulsion, a Solsperse 27000 dispersant, phthalocyanine blue, barium sulfate, talcum powder and water at 50 ℃ and at a stirring speed of 900rpm for 30min, grinding to the fineness of 5 mu m, cooling to 25 ℃, adding the rest components into the premixed system, and then mixing to obtain the waterborne ink.
Example 5
The only difference from example 1 is that 45 parts of the aliphatic polycarbonate type aqueous polyurethane emulsion and 15 parts of the aliphatic polyester type aqueous polyurethane emulsion, that is, the mass ratio of the aliphatic polycarbonate type aqueous polyurethane emulsion to the aliphatic polyester type aqueous polyurethane emulsion is 3: 1.
Example 6
The only difference from example 1 is that 15 parts of the aliphatic polycarbonate type aqueous polyurethane emulsion and 45 parts of the aliphatic polyester type aqueous polyurethane emulsion, that is, the mass ratio of the aliphatic polycarbonate type aqueous polyurethane emulsion to the aliphatic polyester type aqueous polyurethane emulsion is 0.33: 1.
Comparative example 1
The only difference from example 1 is that the aliphatic polyester type aqueous polyurethane emulsion was replaced with an aliphatic polycarbonate type aqueous polyurethane emulsion, that is, 60 parts of the aliphatic polycarbonate type aqueous polyurethane emulsion.
Comparative example 2
The only difference from example 1 is that the aliphatic polycarbonate type aqueous polyurethane emulsion was replaced with an aliphatic polyester type aqueous polyurethane emulsion, that is, 60 parts of an aliphatic polyester type aqueous polyurethane emulsion.
And (3) performance testing:
wet sample test 1:
1. viscosity: the aqueous inks obtained in the examples and comparative examples of the present invention were subjected to viscosity testing in accordance with GB/T13217.4-2008 viscosity test method for liquid inks, and the results are shown in Table 1.
2. Fineness: the water-based inks obtained in examples of the present invention and comparative examples were subjected to fineness tests according to GB/T13217.3-2008 liquid ink fineness test method, and the details of the test structures are shown in Table 1.
TABLE 1
Sample (I) Fineness (mum) Viscosity (cps/25 ℃ C.)
Example 1 ≦5 5300±200
Example 2 ≦5 3600±200
Example 3 ≦5 2800±200
Example 4 ≦5 4800±200
Example 5 ≦5 5200±200
Example 6 ≦5 5100±200
Comparative example 1 ≦5 5400±200
Comparative example 2 ≦5 5000±200
As can be seen from the data in Table 1, the fineness of the inks prepared in the examples of the present invention is less than or equal to 5 μm, and the viscosity at 25 ℃ is in the range of 2800 to 5600cps, which indicates that the inks prepared in the examples of the present invention have suitable coating viscosity and good dispersion stability.
Dry film test 2:
1. preparing a sample:
the isocyanate curing agent and the water-based ink prepared by the embodiment of the invention are used for printing a first layer on the surface of the composite material, drying the first layer at 80 ℃ for 20min, then printing a second layer, drying the second layer at 80 ℃ for 20min, then printing a third layer, and curing the third layer at 90 ℃ for 120min to obtain an ink layer.
The water-based ink prepared by the comparative example is coated on the surface of a composite material, the thickness of a single film layer is 3-5 mu m, and the thickness of a third total film layer is less than or equal to 12 mu m, so that an ink layer is obtained.
2. Testing the dry film performance:
the cured ink layers obtained in the examples and comparative examples were subjected to the following dry film property test.
(1) Film thickness: the ink layers obtained in the examples and comparative examples of the present invention were tested for film thickness using an ultrasonic thickness gauge, and the specific test results are shown in table 2.
(2) Adhesion force: the ink layers obtained in the examples and comparative examples of the present invention were subjected to adhesion test according to GB/T13217.7-2009 liquid ink adhesion fastness test method.
The test method comprises the following steps: using a sharp blade to scribe 10 multiplied by 10 small grids of 1 multiplied by 1mm in a designated area, wherein each scribing line penetrates through the ink to the substrate; the surface fragments are brushed clean by using dust-free cloth or a hairbrush, the small grids are adhered by using 3M610 adhesive paper and are flattened, air bubbles are extruded out, the static pressure is kept for more than 5 seconds, the product is kept still, the single side of the adhesive tape is rapidly pulled up at an angle of 90 degrees, and the adhesive force reaches 4B (the falling area is less than 5 percent).
The specific test results are shown in table 2.
(3) Covering power: the hiding power of the ink, i.e., the OD value, is used to characterize the hiding performance of the ink on the substrate.
The test method comprises the following steps: adjusting the viscosity of the ink to 2000cps/25 deg.C, screen printing with 300 mesh screen, baking at 180 deg.C for 60min, and testing the covering power of the obtained dry paint film by OD value detector (transmission method);
evaluation criteria: the higher the OD value, the better the hiding power.
The specific test results are shown in table 2.
(4) Hardness: the ink layers obtained in the examples and comparative examples of the present invention were subjected to pencil hardness test.
The specific test method is as follows:
selecting pencils with different hardness according to the hardness requirement of a product, cutting the pencils by a pencil sharpener until 4-6mm cylindrical pencil cores are exposed (the pencil cores are not loosened or damaged), holding the pencils to enable the pencils to be vertical to a No. 400 abrasive paper surface, and grinding and scratching the abrasive paper until pencil ends with smooth end surfaces and sharp edges are obtained (the edges are not broken or notched);
secondly, mounting the pencil on a mechanical trolley for scratching the pencil, and screwing a fixing clamp;
thirdly, using a Mitsubishi pencil (the surface is PMMA-4H), drawing 3 lines with the length of 1.0 +/-0.2 cm on the surface of the sample from different directions at an angle of 45 degrees and under the load of 1000g/f, and the speed is 7 mm/s.
Evaluation criteria: after the traces of the pencils are wiped off by an eraser, if the ink surface is scratched or scratched, a pencil with a lower hardness level is selected for continuous testing until no scratch or scratch exists after the test, and the hardness of the selected pencil is the hardness of the product. Such as PMMA 3H 4H OK, wherein PMMA 5H must be scratched or scratched.
The specific test results are shown in table 2.
(5) Temperature shock resistance: the ink layers obtained in the examples and comparative examples of the present invention were subjected to a temperature impact resistance test.
The test method is as follows: the ink layers obtained in the embodiment and the comparative example are placed for 1h at the low temperature of minus 40 +/-2 ℃, then are transferred to the high temperature of 75 +/-2 ℃ within 1min for 1h, the low-temperature placement for 1h and the high-temperature placement for 1h are taken as a cycle, the cycle is repeated for 20 times (40h), and after the ink layers are recovered for 2h at the normal temperature, appearance inspection is carried out, and an adhesion test is carried out.
Evaluation criteria: the appearance is not abnormal, and the coating layer and the printing layer are not peeled off; the adhesive force reaches 4B; no delamination between the individual layered structures can occur.
The specific test results are shown in table 2.
(6) High temperature and high humidity resistance: the ink layers obtained in the examples and comparative examples of the present invention were subjected to a high temperature and high humidity test.
The test method is as follows: the ink layers obtained in the embodiment and the comparative example are placed for 48 hours in an environment with the temperature of 75 +/-2 ℃ and the humidity of 95%, then taken out, placed for at least 2 hours under natural conditions, and the state and the performance of the product are observed for judgment.
Evaluation criteria: the appearance is not abnormal, and the coating layer and the printing layer are not peeled off; the adhesive force reaches 4B; no delamination between the individual layered structures can occur.
The specific test results are shown in table 2.
(7) Boiling in water: the ink layers obtained in the examples and comparative examples of the present invention were subjected to a boiling-water resistance test.
The test method is as follows:
firstly, the ink layers prepared in the embodiment of the invention and the comparative example are respectively boiled in water at 80 ℃ for 30min, and the ink layers can not contact the wall of a boiling water solvent;
secondly, drying the fabric by using a dust-free cloth, recovering the fabric at normal temperature for at least 2 hours, and checking the appearance;
③ scratching hundreds of grids: using a sharp blade to scribe 10 multiplied by 10 small grids of 1 multiplied by 1mm in a set area, wherein each scribing line penetrates through the ink to the substrate;
and fourthly, wiping the surface fragments clean by using dust-free cloth, adhering small grids by using 3M610 gummed paper, flattening, extruding bubbles, performing static pressure for more than 5 seconds, and quickly and vertically pulling up the gummed paper at an angle of 90 degrees.
Evaluation criteria:
1) the appearance is not abnormal, and the coating layer and the printing layer are not peeled off;
2) the adhesive force reaches 4B.
The specific test results are shown in table 2.
TABLE 2
Figure GDA0003487026940000151
Figure GDA0003487026940000161
As can be seen from the data in Table 2, the performance indexes of the ink layers prepared in examples 1 to 4 of the present invention are significantly better than those of the ink layers prepared in comparative examples 1 to 2. The ink layers prepared in the embodiments 1 to 4 of the present invention have high adhesion, high hiding power, good impact resistance and chemical resistance, that is, the aqueous ink of the present invention is prepared by compounding the aliphatic polycarbonate type aqueous polyurethane emulsion and the aliphatic polyester type aqueous polyurethane emulsion, and the two are matched with each other to achieve synergistic interaction, so that each physical and chemical property of the prepared ink layers is significantly improved.
Compared with the embodiment 1, the ink layer prepared by adopting only the aliphatic polycarbonate type waterborne polyurethane emulsion in the comparative example 1 and only the aliphatic polyester type waterborne polyurethane emulsion in the comparative example 2 is obviously inferior to the ink layer prepared by the embodiment 1 in various performances, which shows that the performances of the prepared ink layer can be completely improved only by reasonably compounding the aliphatic polycarbonate type waterborne polyurethane emulsion and the aliphatic polyester type waterborne polyurethane emulsion disclosed by the invention, and the two are matched with each other to realize synergistic interaction.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.

Claims (30)

1. The water-based ink is characterized by comprising the following components in parts by weight: 20-70 parts of waterborne polyurethane emulsion, 0.1-2 parts of dispersant, 5-20 parts of pigment, 10-40 parts of filler, 1-5 parts of assistant and 10-30 parts of water; the aqueous polyurethane emulsion comprises aliphatic polycarbonate type aqueous polyurethane emulsion and aliphatic polyester type aqueous polyurethane emulsion;
the viscosity of the aliphatic polycarbonate type aqueous polyurethane emulsion is less than 250mPa ∙ s;
the pH value of the aliphatic polycarbonate type waterborne polyurethane emulsion is 8.5-9.5;
the tensile strength of the aliphatic polycarbonate type waterborne polyurethane emulsion after the polyurethane film forming is 15-20N/mm2；
The elongation at break of the aliphatic polycarbonate type aqueous polyurethane emulsion after the polyurethane film is formed is 300-500%;
the viscosity of the aliphatic polyester type waterborne polyurethane emulsion is less than 500mPa ∙ s;
the pH value of the aliphatic polyester type waterborne polyurethane emulsion is 8.5-9.5;
the tensile strength of the polyurethane in the aliphatic polyester type waterborne polyurethane emulsion after film formation is 15-20N/mm2；
The elongation at break of the aliphatic polyester type waterborne polyurethane emulsion after film formation of polyurethane is 500-700%;
the mass ratio of the aliphatic polycarbonate type aqueous polyurethane emulsion to the aliphatic polyester type aqueous polyurethane emulsion is (0.5-2) to 1.
2. The water-based ink as claimed in claim 1, wherein the water-based ink comprises the following components in parts by weight: 20-50 parts of aqueous polyurethane emulsion, 0.1-2 parts of dispersant, 5-15 parts of pigment, 10-40 parts of filler, 1-5 parts of assistant and 10-30 parts of water.
3. The aqueous ink according to claim 1, wherein the aliphatic polycarbonate-based aqueous polyurethane emulsion and the aliphatic polyester-based aqueous polyurethane emulsion are in a mass ratio of 1: 1.
4. The aqueous ink according to claim 1, wherein the aliphatic polycarbonate-based aqueous polyurethane emulsion has a solid content of 25 to 35%.
5. The aqueous ink according to claim 1, wherein the aliphatic polyester-based aqueous polyurethane emulsion has a solid content of 30 to 40%.
6. The aqueous ink of claim 1, wherein the dispersant is Solsperse 27000.
7. The aqueous ink according to claim 1, wherein the pigment is selected from any one of carbon black, titanium dioxide, aniline yellow, phthalocyanine blue or ultramarine blue or a combination of at least two of the above.
8. The aqueous ink of claim 1, wherein the filler comprises any one of barium sulfate, talc, or alumina powder, or a combination of at least two thereof.
9. The aqueous ink according to claim 1, wherein the assistant comprises 0.1 to 0.5 parts of a leveling agent.
10. The aqueous ink according to claim 9, wherein the leveling agent is an acrylate-based leveling agent.
11. The aqueous ink of claim 10, wherein the leveling agent is BYK-3560 and/or BYK-3565.
12. The aqueous ink according to claim 1, wherein the auxiliary further comprises 0.1 to 1 part of a pH stabilizer.
13. The aqueous ink of claim 12, wherein the pH stabilizer is AMP-95.
14. The aqueous ink according to claim 1, wherein the auxiliary further comprises 0.1 to 0.5 parts of a bactericide.
15. The aqueous ink of claim 14, wherein the biocide is KATHON LXE.
16. The aqueous ink of claim 1, wherein the adjuvant further comprises 1 to 3 parts of a defoamer.
17. The aqueous ink according to claim 16, wherein the defoaming agent is a non-silicone defoaming agent.
18. The aqueous ink of claim 17, wherein the defoamer is BYK-015 and/or BYK-1710.
19. A method for preparing an aqueous ink according to any one of claims 1 to 18, comprising: and mixing the aqueous polyurethane emulsion, a dispersant, a pigment, water, a filler and an auxiliary agent to obtain the aqueous ink.
20. The method of claim 19, wherein the mixing is performed by: premixing the aqueous polyurethane emulsion, the dispersant, the pigment, the water and the pigment, adding the auxiliary agent into the premixed system, and then mixing.
21. The method of claim 20, wherein the temperature of the pre-mixing is 40-60 ℃.
22. The method according to claim 20, wherein the time for the premixing is 30min or more.
23. The method of claim 22, wherein the pre-mixing time is 60-120 min.
24. The method as claimed in claim 20, wherein the pre-mixing is performed at a stirring speed of 300-1000 rpm.
25. The method as claimed in claim 24, wherein the pre-mixing is performed at a stirring speed of 500-700 rpm.
26. The method as claimed in claim 20, wherein the premixed system is ground to a fineness of 5 μm or less before the addition of the auxiliary.
27. The method of claim 20, wherein the premixed system is cooled to 18-30 ℃ before the addition of the adjuvant.
28. An ink layer obtained by curing a curing agent and the aqueous ink according to any one of claims 1 to 18.
29. A method for preparing the ink layer according to claim 28, wherein the method comprises: and mixing the water-based ink and a curing agent, printing a first layer on the surface of the base material by using the obtained mixture, drying the surface, then printing a second layer, drying the surface, repeating the printing and drying process, printing an Nth layer, drying the surface and curing to obtain the ink layer.
30. Use of an aqueous ink according to any one of claims 1 to 18 in a polycarbonate ink, a polyethylene terephthalate ink or a composite ink.
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