CN104629531A - Nano-aluminum-oxide-modified composite water-based ink and preparation method thereof - Google Patents
Nano-aluminum-oxide-modified composite water-based ink and preparation method thereof Download PDFInfo
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- CN104629531A CN104629531A CN201510019712.2A CN201510019712A CN104629531A CN 104629531 A CN104629531 A CN 104629531A CN 201510019712 A CN201510019712 A CN 201510019712A CN 104629531 A CN104629531 A CN 104629531A
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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
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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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
- C09D11/104—Polyesters
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- Inks, Pencil-Leads, Or Crayons (AREA)
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Abstract
The invention belongs to the field of water-based inks, and discloses a nano-aluminum-oxide-modified composite water-based ink which is composed of a nano-aluminum-oxide-modified water-based acrylic resin, a water-based polyester resin, water, ethanol, a pigment, a defoaming agent, a dispersing agent, a leveling agent and a buffer agent. The preparation process comprises the following steps: preparing silane coupling agent modified inorganic nanoparticles from nano aluminum oxide, ethanol, water and gamma-methylacryloyloxypropyltrimethoxy silane; preparing the nano-aluminum-oxide-modified water-based acrylic resin from an alkyl acrylate monomer, a hydroxyalkyl acrylate monomer, the silane coupling agent modified inorganic nanoparticles, polyethyleneglycol, a water-soluble initiator, an emulsifier and water; and finally, preparing the nano-aluminum-oxide-modified composite water-based ink from the nano-aluminum-oxide-modified water-based acrylic resin, a water-based polyester resin, water, ethanol, a pigment, a defoaming agent, a dispersing agent, a leveling agent and a buffer agent. The water-based ink has excellent wearability and chemical resistance.
Description
Technical field
The present invention relates to water color ink field, particularly relate to Compound waterborne ink of a kind of nano-aluminium oxide modification and preparation method thereof.
Background technology
Water color ink take water as the ink that solvent is made, and is prepared from through physical and chemical process combination by specific aqueous high molecular resin, pigment, water and solubility promoter etc.Compared oiliness and machine solvent type ink, water color ink can not cause the volatilization of a large amount of organic solvent, and toxicity is low, little on the healthy impact of direct labor, and more and more paying attention to today of environment protection and health of human body, water color ink has huge development prospect.But the development due to water color ink does not have the full-fledged of solvent type ink, Shortcomings in many performances.
Authorization Notice No. CN 102040884 B, the authorized announcement date Chinese invention patent of on 03 20th, 2013 discloses a kind of alcohol aqueous composite ink formula, be made into by water-borne acrylic resin, nitro-cotton, dispersion agent, scratch resistance agent, dumb light powder, flow agent, defoamer, pigment, ethanol, Virahol, methyl ether and deionized water, this ink employs water-borne acrylic resin, using deionized water and alcohols as solvent, break away from the shortcoming that the benzene molten type chlorinated polypropylene of conventional composite ink is large to human injury, decrease the discharge of VOC simultaneously, reduce cost.The weak point of this invention is: although add scratch resistance agent, and the scratch resistance agent just added when preparing cannot from the wear resisting property improving water-borne acrylic resin itself, weak effect, simultaneously the chemical resistance also Shortcomings of ink.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides Compound waterborne ink of a kind of nano-aluminium oxide modification and preparation method thereof.The water color ink prepared by the inventive method not only environmental protection, and there is excellent wear resisting property and chemical resistance.
Concrete technical scheme of the present invention is: a kind of Compound waterborne ink of nano-aluminium oxide modification, and by weight percentage, its each component concentration is as follows:
Nano-aluminium oxide modified aqueous acrylic acid resin 20-30wt%; Aqueous polyester resin 15-20 wt%; Water 20-30 wt%; Ethanol 5-15 wt%; Pigment 10-30 wt%; Defoamer 0.5-1.5 wt%; Dispersion agent 1-2 wt%; Flow agent 1-2 wt%; Buffer reagent 1-2 wt%.
As preferably, the formula of the Compound waterborne ink of nano-aluminium oxide modification is:
Nano-aluminium oxide modified aqueous acrylic acid resin 25wt%; Aqueous polyester resin 17.5 wt%; Water 24 wt%; Ethanol 8wt%; Pigment 20 wt%; Defoamer 1 wt%; Dispersion agent 1.5 wt%; Flow agent 1.5 wt%; Buffer reagent 1.5 wt%.
Present invention also offers a kind of preparation method of Compound waterborne ink of above-mentioned nano-aluminium oxide modification, carry out as follows:
(1) at 60 DEG C of water-bath back flow reaction 8-16h after nano-aluminium oxide, ethanol, water and γ-methacryloxypropyl trimethoxy silane being mixed, then room temperature is down to, product is through centrifugation and washing, obtain silane coupler modified inorganic nano-particle, the weight consumption of described nano-aluminium oxide, ethanol, water and γ-methacryloxypropyl trimethoxy silane is than being 1:30-50:5-15:1-3.
(2) 30-60 part water and 1-3 part emulsifying agent are put into reactor and be heated to 80 DEG C, again by 20-35 part alkyl acrylate monomer, 10-20 part hydroxyalkyl acrylates monomer, the silane coupler modified inorganic nano-particle of 5-10 part step (1) gained, stir after 3-5 part polyoxyethylene glycol and 0.25-0.5 part water soluble starter put into reactor, be incubated after 0.5-1 hour, 0.25-0.5 part water soluble starter is at the uniform velocity added in 2 hours, and then filtration obtains nano-aluminium oxide modified aqueous acrylic acid resin after being incubated 4-8 hour, above material number is parts by weight.
(3) the nano-aluminium oxide modified aqueous acrylic acid resin of step (2) gained is mixed by proportioning with aqueous polyester resin, water, ethanol, pigment, defoamer, dispersion agent, flow agent, buffer reagent, then obtain the Compound waterborne ink of nano-aluminium oxide modification by grinding distribution.
As preferably, the particle diameter of described nano-aluminium oxide is at 10-40nm.
As preferably, described alkyl acrylate monomer is methyl methacrylate, β-dimethyl-aminoethylmethacrylate or butyl acrylate; Described hydroxyalkyl acrylates monomer is hydroxyethyl methylacrylate or Rocryl 410.
Be compared with the prior art, the invention has the beneficial effects as follows: the inventive method introduces hydrophilic-structure by polyoxyethylene glycol, improve the wetting ability of acrylic resin, water-borne acrylic resin and aqueous polyester resin being carried out composite is that water color ink prepared by primary solvent with water, greatly reduce the usage quantity of organic solvent, environmental protection, low to human injury.
Simultaneously, silane coupling agent is adopted to carry out modification to nano-aluminium oxide, can with acrylate monomer copolymerization, nano-aluminium oxide and hydroxyalkyl are incorporated on water-borne acrylic resin, nano-aluminium oxide after modified participates in polymerization directly, being evenly distributed in resin, better to the modified effect of water-borne acrylic resin, with the water color ink that water-borne acrylic resin is main binder, chemical resistant properties after printing and wear resisting property obtain great lifting.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
(1) preparation of silane coupler modified inorganic nano-particle
At 60 DEG C of water-bath back flow reaction 8h after the nano-aluminium oxide, ethanol, water and the γ-methacryloxypropyl trimethoxy silane that are 1:30:5:1 by weight consumption ratio mix, then room temperature is down to, product, through centrifugation and washing, obtains silane coupler modified inorganic nano-particle.The particle diameter of described nano-aluminium oxide is 10nm.
(2) preparation of nano-aluminium oxide modified aqueous acrylic acid resin
30 parts of water and 1 part of emulsifying agent are put into reactor and is heated to 80 DEG C, again by the silane coupler modified inorganic nano-particle of 20 parts of methyl methacrylates, 10 parts of hydroxyethyl methylacrylates, 5 parts of step (1) gained, stir after 3 parts of polyoxyethylene glycol and 0.25 part of water soluble starter put into reactor, be incubated after 0.5 hour, in 2 hours, at the uniform velocity add 0.25 part of water soluble starter, and then after being incubated 4 hours, filtration obtains nano-aluminium oxide modified aqueous acrylic acid resin.
(3) preparation of the Compound waterborne ink of nano-aluminium oxide modification
The each component concentration of Compound waterborne ink of nano-aluminium oxide modification is as follows:
Nano-aluminium oxide modified aqueous acrylic acid resin 20wt%;
Aqueous polyester resin 20 wt%;
Water 25 wt%;
Ethanol 10wt%;
Pigment 20 wt%;
Defoamer 0.5 wt%;
Dispersion agent 1.5 wt%;
Flow agent 1.5 wt%;
Buffer reagent 1.5 wt%.
The nano-aluminium oxide modified aqueous acrylic acid resin of step (2) gained is mixed by proportioning with aqueous polyester resin, water, ethanol, pigment, defoamer, dispersion agent, flow agent, buffer reagent, more namely obtains the Compound waterborne ink of nano-aluminium oxide modification by grinding distribution.
Embodiment 2
(1) preparation of silane coupler modified inorganic nano-particle
At 60 DEG C of water-bath back flow reaction 16h after the nano-aluminium oxide, ethanol, water and the γ-methacryloxypropyl trimethoxy silane that are 1:50:15:3 by weight consumption ratio mix, then room temperature is down to, product, through centrifugation and washing, obtains silane coupler modified inorganic nano-particle.The particle diameter of described nano-aluminium oxide is 20nm.
(2) preparation of nano-aluminium oxide modified aqueous acrylic acid resin
60 parts of water and 3 parts of emulsifying agents are put into reactor and is heated to 80 DEG C, again by the silane coupler modified inorganic nano-particle of 35 parts of butyl acrylates, 20 parts of Rocryl 410s, 10 parts of step (1) gained, stir after 5 parts of polyoxyethylene glycol and 0.5 part of water soluble starter put into reactor, be incubated after 1 hour, in 2 hours, at the uniform velocity add 0.5 part of water soluble starter, and then after being incubated 8 hours, filtration obtains nano-aluminium oxide modified aqueous acrylic acid resin.
(3) preparation of the Compound waterborne ink of nano-aluminium oxide modification
The each component concentration of Compound waterborne ink of nano-aluminium oxide modification is as follows:
Nano-aluminium oxide modified aqueous acrylic acid resin 25wt%;
Aqueous polyester resin 17.5wt%;
Water 24 wt%;
Ethanol 8wt%;
Pigment 20 wt%;
Defoamer 1 wt%;
Dispersion agent 1.5 wt%;
Flow agent 1.5 wt%;
Buffer reagent 1.5 wt%.
The nano-aluminium oxide modified aqueous acrylic acid resin of step (2) gained is mixed by proportioning with aqueous polyester resin, water, ethanol, pigment, defoamer, dispersion agent, flow agent, buffer reagent, more namely obtains the Compound waterborne ink of nano-aluminium oxide modification by grinding distribution.
Embodiment 3
(1) preparation of silane coupler modified inorganic nano-particle
At 60 DEG C of water-bath back flow reaction 12h after the nano-aluminium oxide, ethanol, water and the γ-methacryloxypropyl trimethoxy silane that are 1:40:10:2 by weight consumption ratio mix, then room temperature is down to, product, through centrifugation and washing, obtains silane coupler modified inorganic nano-particle.The particle diameter of described nano-aluminium oxide is 40nm.
(2) preparation of nano-aluminium oxide modified aqueous acrylic acid resin
45 parts of water and 2 parts of emulsifying agents are put into reactor and is heated to 80 DEG C, again by the silane coupler modified inorganic nano-particle of 27.5 parts of β-dimethyl-aminoethylmethacrylates, 15 parts of Rocryl 410s, 7.5 parts of step (1) gained, stir after 4 parts of polyoxyethylene glycol and 0.4 part of water soluble starter put into reactor, be incubated after 1 hour, in 2 hours, at the uniform velocity add 0.4 part of water soluble starter, and then after being incubated 6 hours, filtration obtains nano-aluminium oxide modified aqueous acrylic acid resin.
(3) preparation of the Compound waterborne ink of nano-aluminium oxide modification
The each component concentration of Compound waterborne ink of nano-aluminium oxide modification is as follows:
Nano-aluminium oxide modified aqueous acrylic acid resin 30wt%;
Aqueous polyester resin 15wt%;
Water 22.5wt%;
Ethanol 15wt%;
Pigment 10 wt%;
Defoamer 1.5 wt%;
Dispersion agent 2wt%;
Flow agent 2 wt%;
Buffer reagent 2 wt%.
The nano-aluminium oxide modified aqueous acrylic acid resin of step (2) gained is mixed by proportioning with aqueous polyester resin, water, ethanol, pigment, defoamer, dispersion agent, flow agent, buffer reagent, more namely obtains the Compound waterborne ink of nano-aluminium oxide modification by grinding distribution.
Embodiment 4
(1) preparation of silane coupler modified inorganic nano-particle
At 60 DEG C of water-bath back flow reaction 10h after the nano-aluminium oxide, ethanol, water and the γ-methacryloxypropyl trimethoxy silane that are 1:40:8:2.5 by weight consumption ratio mix, then room temperature is down to, product, through centrifugation and washing, obtains silane coupler modified inorganic nano-particle.The particle diameter of described nano-aluminium oxide is 25nm.
(2) preparation of nano-aluminium oxide modified aqueous acrylic acid resin
50 parts of water and 2.5 parts of emulsifying agents are put into reactor and is heated to 80 DEG C, again by the silane coupler modified inorganic nano-particle of 30 parts of methyl methacrylates, 15 parts of hydroxyethyl methylacrylates, 6 parts of step (1) gained, stir after 4 parts of polyoxyethylene glycol and 0.3 part of water soluble starter put into reactor, be incubated after 0.75 hour, in 2 hours, at the uniform velocity add 0.3 part of water soluble starter, and then after being incubated 7 hours, filtration obtains nano-aluminium oxide modified aqueous acrylic acid resin.
(3) preparation of the Compound waterborne ink of nano-aluminium oxide modification
The each component concentration of Compound waterborne ink of nano-aluminium oxide modification is as follows:
Nano-aluminium oxide modified aqueous acrylic acid resin 25wt%;
Aqueous polyester resin 18wt%;
Water 20 wt%;
Ethanol 10wt%;
Pigment 22.5 wt%;
Defoamer 1.5wt%;
Dispersion agent 1 wt%;
Flow agent 1 wt%;
Buffer reagent 1wt%.
The nano-aluminium oxide modified aqueous acrylic acid resin of step (2) gained is mixed by proportioning with aqueous polyester resin, water, ethanol, pigment, defoamer, dispersion agent, flow agent, buffer reagent, more namely obtains the Compound waterborne ink of nano-aluminium oxide modification by grinding distribution.
The above; it is only preferred embodiment of the present invention; not the present invention is imposed any restrictions, every above embodiment is done according to the technology of the present invention essence any simple modification, change and equivalent transformation, all still belong to the protection domain of technical solution of the present invention.
Claims (5)
1. a Compound waterborne ink for nano-aluminium oxide modification, is characterized in that by weight percentage, and its each component concentration is as follows:
Nano-aluminium oxide modified aqueous acrylic acid resin 20-30wt%;
Aqueous polyester resin 15-20 wt%;
Water 20-30 wt%;
Ethanol 5-15 wt%;
Pigment 10-30 wt%;
Defoamer 0.5-1.5 wt%;
Dispersion agent 1-2 wt%;
Flow agent 1-2 wt%;
Buffer reagent 1-2 wt%.
2. the Compound waterborne ink of nano-aluminium oxide modification as claimed in claim 1, it is characterized in that by weight percentage, its each component concentration is as follows:
Nano-aluminium oxide modified aqueous acrylic acid resin 25wt%;
Aqueous polyester resin 17.5 wt%;
Water 24wt%;
Ethanol 8wt%;
Pigment 20 wt%;
Defoamer 1 wt%;
Dispersion agent 1.5 wt%;
Flow agent 1.5 wt%;
Buffer reagent 1.5 wt%.
3. a preparation method for the Compound waterborne ink of nano-aluminium oxide modification as claimed in claim 1 or 2, is characterized in that carrying out as follows:
(1) at 60 DEG C of water-bath back flow reaction 8-16h after nano-aluminium oxide, ethanol, water and γ-methacryloxypropyl trimethoxy silane being mixed, then room temperature is down to, product is through centrifugation and washing, obtain silane coupler modified inorganic nano-particle, the weight consumption of described nano-aluminium oxide, ethanol, water and γ-methacryloxypropyl trimethoxy silane is than being 1:30-50:5-15:1-3;
(2) 30-60 part water and 1-3 part emulsifying agent are put into reactor and be heated to 80 DEG C, again by 20-35 part alkyl acrylate monomer, 10-20 part hydroxyalkyl acrylates monomer, the silane coupler modified inorganic nano-particle of 5-10 part step (1) gained, stir after 3-5 part polyoxyethylene glycol and 0.25-0.5 part water soluble starter put into reactor, be incubated after 0.5-1 hour, 0.25-0.5 part water soluble starter is at the uniform velocity added in 2 hours, and then filtration obtains nano-aluminium oxide modified aqueous acrylic acid resin after being incubated 4-8 hour, above material number is parts by weight,
(3) the nano-aluminium oxide modified aqueous acrylic acid resin of step (2) gained is mixed by proportioning with aqueous polyester resin, water, ethanol, pigment, defoamer, dispersion agent, flow agent, buffer reagent, then obtain the Compound waterborne ink of nano-aluminium oxide modification by grinding distribution.
4. the preparation method of the Compound waterborne ink of nano-aluminium oxide modification as claimed in claim 3, it is characterized in that, the particle diameter of described nano-aluminium oxide is at 10-40nm.
5. the preparation method of the Compound waterborne ink of nano-aluminium oxide modification as claimed in claim 3, it is characterized in that, described alkyl acrylate monomer is methyl methacrylate, β-dimethyl-aminoethylmethacrylate or butyl acrylate; Described hydroxyalkyl acrylates monomer is hydroxyethyl methylacrylate or Rocryl 410.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437131A (en) * | 2018-12-27 | 2019-03-08 | 沈阳金瓷科技开发有限责任公司 | Method based on the modified low temperature synthesis aluminum nitride ceramic powder in surface |
| CN112940601A (en) * | 2019-11-26 | 2021-06-11 | 广州四面体新材料科技有限公司 | Ultraviolet curing coating for enhancing wear resistance and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101108946A (en) * | 2007-07-12 | 2008-01-23 | 深圳清华大学研究院 | Nano transparent insulating paint and its preparing process |
| CN104263069A (en) * | 2014-08-29 | 2015-01-07 | 湖南新力华纳米科技有限公司 | Water-based thermosetting glass printing ink and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101108946A (en) * | 2007-07-12 | 2008-01-23 | 深圳清华大学研究院 | Nano transparent insulating paint and its preparing process |
| CN104263069A (en) * | 2014-08-29 | 2015-01-07 | 湖南新力华纳米科技有限公司 | Water-based thermosetting glass printing ink and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437131A (en) * | 2018-12-27 | 2019-03-08 | 沈阳金瓷科技开发有限责任公司 | Method based on the modified low temperature synthesis aluminum nitride ceramic powder in surface |
| CN112940601A (en) * | 2019-11-26 | 2021-06-11 | 广州四面体新材料科技有限公司 | Ultraviolet curing coating for enhancing wear resistance and preparation method thereof |
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