CN110669383A - Preparation method of nano material for improving ultraviolet performance of PET food packaging ink-jet coating - Google Patents
Preparation method of nano material for improving ultraviolet performance of PET food packaging ink-jet coating Download PDFInfo
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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
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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Abstract
The invention discloses a preparation method of a nano material for improving ultraviolet performance of an ink-jet coating of PET food packaging, which comprises the following steps: step one, coating zinc oxide ZnO @ SiO with silicon dioxide2Preparing; step two, pigment ZnO @ SiO2Preparing the dispersion of (4); step three, preparing and coating the ink-jet coating liquid. The invention takes quantum dot ZnO as a core and SiO2The shell is used for preparing UV-A ultraviolet resistant nano particles, and the UV-A ultraviolet resistant nano particles are used as pigments, PET films are used as base materials, and polyvinyl alcohol is used as an adhesive, so that the UV-A ultraviolet resistant nano particles with excellent performance are obtainedThe PET food packaging film has different ultraviolet resistance, good ink spraying performance and can shield most of UV-A ultraviolet light. ZnO @ SiO prepared by the invention2Nanoparticles compared to commercial SiO2Has higher porosity, thus greatly improving the ink absorption performance of the coating.
Description
Technical Field
The invention relates to a preparation method of a PET food packaging ink-jet coating nano material resistant to UV-A ultraviolet light.
Background
Ultraviolet radiation is radiation from the sun, the wavelength range of which is 200 ~ 400nm, wherein the high-energy short wave energy below 290 nm is almost completely absorbed by the atmosphere, and the wavelength of the ultraviolet radiation finally reaching the ground is about 290 ~ 400nm, wherein the ultraviolet radiation of 290 ~ 320 nm only accounts for 8 percent of the total ultraviolet radiation reaching the ground, and most of the ultraviolet radiation is ultraviolet radiation in the UV-A (320 ~ 400 nm) wave band.
Various transparent PET food packaging bags used in daily life are not qualified, and are directly irradiated by ultraviolet rays, so that food is deteriorated and seriously harms human health, and the transmittance of the transparent PET food packaging bags to the ultraviolet rays directly influences the human health. In order to solve the problem, various ultraviolet shielding agents appear in the modern society, the ultraviolet shielding problem becomes a topic which is objected to in the contemporary scientific community, and the ultraviolet shielding agents have wide application prospects.
At present, ultraviolet screening agents are mainly divided into organic screening agents and inorganic screening agents. The shielding performance of the organic shielding agent is gradually reduced along with the irradiation of ultraviolet light and has strong toxicity, which can substantially affect the ultraviolet shielding performance of the film. Inorganic ultraviolet shielding agents such as titanium dioxide, zinc oxide and the like have excellent ultraviolet shielding performance, but the phenomenon of photocatalytic degradation can occur, so that the performance of a packaging coating is reduced, and particularly, after long-time illumination, character images printed by ink jet on the surface of a packaging film become fuzzy, so that the application of a packaging material is influenced. And these inorganic uv screeners do not have the ink receptivity required for inkjet printing, further limiting the application of the material.
Disclosure of Invention
In order to solve the problems of poor UV-A ultraviolet resistance and poor ink-jet printing performance of the conventional transparent PET food packaging film, the invention provides a preparation method of a nano material for improving the ultraviolet performance of an ink-jet coating of PET food packaging. The invention takes quantum dot ZnO as a core and SiO2The PET food packaging film has excellent ultraviolet resistance, good ink spraying performance and can shield most of UV-A ultraviolet light.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a nano material for improving the ultraviolet performance of a PET food packaging coating comprises the following steps:
step one, preparation of a quantum dot zinc oxide solution:
(1) anhydrous zinc acetate (Zn (Ac)2) Dissolving: taking 1 mol of Zn (Ac)2Dispersing the mixture into 30 ~ 50mL of absolute ethyl alcohol, gradually heating to 75 ~ 80 ℃, and dispersing and dissolving for 2 ~ 3 h;
(2) dissolving sodium hydroxide (NaOH), namely taking 1 ~ 3 mol of NaOH, dispersing the NaOH in 10 ~ 30mL of absolute ethyl alcohol, and carrying out ultrasonic treatment for 10 ~ 20min under the power of 480W until the NaOH is dissolved;
(3) reacting Zn (Ac) in the step (1)2Mixing the solution with the NaOH solution in the step (2) according to the molar ratio of 1:1 ~ 3, stirring at room temperature, and reacting for 1.5 ~ 3 h;
step two, coating zinc oxide (ZnO @ SiO) by silicon dioxide2) The preparation of (1):
(1) adding tetraethoxysilane into the stirring quantum dot zinc oxide solution according to the molar ratio of Zn atoms to Si atoms of 1:1 ~ 3, and then adding water into the stirring quantum dot zinc oxide solution according to the molar ratio of tetraethoxysilane to water of 1:4 ~ 8;
(2) stirring for 24 ~ 30h, and stopping stirring until precipitate is generated;
(3) centrifuging and washing the product at 9000 ~ 10000rmp/min for 3 ~ 4 times (10 min each), collecting the product, and freeze drying;
step three, pigment ZnO @ SiO2Preparation of the dispersion of (4):
the ZnO @ SiO obtained in the second step2Dispersing in a certain amount of water, and dispersing at high speed with homogenizing emulsifier to obtain uniformly dispersed dispersion, i.e. pigment ZnO @ SiO2The dispersion of (1);
step four, preparing and coating the ink-jet coating liquid:
(1) taking 10 ~ 30 parts of 2 ~ 20wt% PVA solution and 10 parts of pigment ZnO @ SiO270 ~ parts of the dispersion liquid, 1 ~ parts of boric acid and 5 ~ parts of ethanol are mixed and dispersed at high speed for 40 ~ min under a homogenizing emulsifying machine, and then the uniformly dispersed ink-jet coating liquid can be obtained;
(2) and (3) taking the PET film with a clean surface, coating the ink-jet coating liquid by using a coating machine, and then drying in an oven at 75 ~ 90 ℃ to obtain the PET film with the ink-jet coating.
Compared with the prior art, the invention has the following advantages:
1. introduction of ZnO quantum dots: the ZnO quantum dots can absorb most of ultraviolet light in the UV-A wave band, when the nano particles are used as the pigment of the ink-jet coating, the ZnO quantum dots can play the advantage of shielding the UV-A ultraviolet light, and when the coating is applied to the field of food packaging, the phenomenon that food is deteriorated due to ultraviolet radiation can be effectively prevented, so that the quality guarantee period of the food is prolonged.
2、SiO2Coating ZnO quantum dots: when the ZnO quantum dot is used alone as an ultraviolet shielding agent, the ultraviolet can be shielded, and the photocatalytic degradation effect of the ultraviolet on the ZnO quantum dot, namely SiO, can not be avoided2The coating of ZnO quantum dots greatly reduces the photocatalytic degradation effect. ZnO @ SiO2When used as ink-jet coating pigment, the pigment avoids the reduction of printing effect caused by photodegradation, and can be applied to jet printingAnd (4) ink printing.
3. ZnO and SiO2The combination of (1): ZnO @ SiO prepared by the invention2Nanoparticles compared to commercial SiO2Has higher porosity, thus greatly improving the ink absorption performance of the coating.
Drawings
FIG. 1 is a commercial SiO2(A-200) nanoparticles and the pigment ZnO @ SiO prepared by the invention2Nitrogen adsorption and desorption curves for nanoparticles.
FIG. 2 shows ZnO quantum dots and ZnO @ SiO2Degradation of nanoparticles under 365nm ultraviolet light (with rhodamine B as a dye), a: ZnO quantum dots, b: ZnO @ SiO2Nanoparticles.
FIG. 3 shows a simple PET film, a PVA coating and the addition of ZnO @ SiO2Uv transmission spectrum of PVA coating of nanoparticles.
Detailed Description
The technical solution of the present invention is further described below with reference to the accompanying drawings, but not limited thereto, and any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention shall be covered by the protection scope of the present invention.
The first embodiment is as follows: the embodiment provides a preparation method of a nano composite ink absorption material, which specifically comprises the following steps:
step one, preparation of a quantum dot zinc oxide solution:
(1) anhydrous zinc acetate (Zn (Ac)2) Dissolving: taking 1 mol of Zn (Ac)2Dispersing the mixture into 30 ~ 50mL of absolute ethyl alcohol, gradually heating to 75 ~ 80 ℃, and dispersing and dissolving for 2 ~ 3 h;
(2) dissolving sodium hydroxide (NaOH) 1 ~ 2 mol of NaOH (nZn (Ac)2nNaOH =1:1 ~ 2), dispersing in 10 ~ 30mL of absolute ethyl alcohol, and carrying out ultrasonic treatment for 10 ~ 20min under 480W of power until NaOH is dissolved;
(3) reacting Zn (Ac) in the step (1)2Mixing the solution with the NaOH solution in the step (2), placing the mixture at room temperature for stirring, and reacting the mixture 1.5 ~ 3 h；
Step two, coating zinc oxide (ZnO @ SiO) by silicon dioxide2) The preparation of (1):
(1) adding 1 ~ 2 parts by mole of tetraethoxysilane into a stirring quantum dot zinc oxide solution according to the mole ratio of Zn atoms to Si atoms of 1:1 ~ 2, and then adding 4 ~ 8 parts of water according to the mole ratio of tetraethoxysilane to water of 1:4 ~ 8;
(2) stirring for 24 ~ 30h, and stopping stirring until precipitate is generated;
(3) centrifuging and washing the product at 9000 ~ 10000rmp/min for 3 ~ 4 times (10 min each), collecting the product, and freeze drying;
step three, pigment ZnO @ SiO2Preparation of the dispersion of (4):
the ZnO @ SiO obtained in the second step2Dispersing in a certain amount of water, and dispersing at high speed with homogenizing emulsifier to obtain uniformly dispersed dispersion, i.e. pigment ZnO @ SiO2The dispersion of (1);
step four, preparing and coating the ink-jet coating liquid:
(1) taking 10 ~ 20 parts of 2 ~ 10wt% PVA solution and 10 parts of pigment ZnO @ SiO 280 ~ parts of the dispersion liquid, 1 ~ parts of boric acid and 5 ~ parts of ethanol are mixed, and high-speed dispersion is carried out for 40 ~ min under a homogenizing emulsifying machine, so as to obtain uniformly dispersed ink-jet coating liquid;
(2) and (3) taking the PET film with a clean surface, coating the ink-jet coating liquid by using a coating machine, and then drying in an oven at 75 ~ 90 ℃ to obtain the PET film with the ink-jet coating.
The nano composite ink absorbing material synthesized by the embodiment has good ultraviolet shielding performance, can block most of ultraviolet light in the UV-A wave band, and is due to SiO2The quantum dot ZnO is coated, so that the photocatalytic degradation effect of zinc oxide can be effectively reduced, and the prepared ZnO @ SiO is prepared2Has higher porosity, has excellent ink absorption performance and can be applied to ink jet printing.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: in the first step, anhydrous Zn (Ac)2The molar ratio to NaOH was 1:2 ~ 3.
Third embodiment the present embodiment is different from the first embodiment in that 2 ~ 3 parts of ethyl orthosilicate is added to the zinc oxide solution being stirred in the second step in a molar ratio of Zn atoms to Si atoms of 1:2 ~ 3.
Fourth embodiment the difference between the first embodiment and the second embodiment is that in the fourth step, 10 ~ 20 parts by weight of 11 ~ 20wt% PVA solution are taken.
Fifth specific embodiment the difference between the first specific embodiment and the second specific embodiment is that in the fourth step, 20 ~ 30 parts of 2 ~ 10wt% PVA solution and 20 parts of pigment ZnO @ SiO270 ~ 80 parts of dispersion liquid.
The following examples were used to demonstrate the beneficial effects of the present invention:
example (b):
step one, preparation of a quantum dot zinc oxide solution:
(1) anhydrous zinc acetate (Zn (Ac)2) Dissolving: taking 1 mol of Zn (Ac)2Dispersing the mixture in 40mL of absolute ethyl alcohol, gradually heating to 79 ℃, and dispersing and dissolving for 3 hours;
(2) dissolution of sodium hydroxide (NaOH): 2 mol of NaOH (nZn (Ac) are taken2: nNaOH =1: 2), dispersing the mixture in 20mL of absolute ethanol, and performing ultrasonic treatment for 10min at 480W power until NaOH is dissolved;
(3) reacting Zn (Ac) in the step (1)2Mixing the solution with the NaOH solution in the step (2), placing the mixture at room temperature, stirring, and reacting for 2 hours;
step two, coating zinc oxide (ZnO @ SiO) by silicon dioxide2) The preparation of (1):
(1) adding 1 part by mole of tetraethoxysilane into a stirring quantum dot zinc oxide solution according to the molar ratio of Zn atoms to Si atoms being 1:1, and then adding 6 parts by mole of water into the tetraethoxysilane and water according to the molar ratio of tetraethoxysilane to water being 1: 6;
(2) stirring for 24h, and stopping stirring until a precipitate is generated;
(3) centrifuging and washing the product at 10000rmp/min for 10min for 3 times, collecting the product, and freeze-drying;
step three, pigment ZnO @ SiO2Preparation of the dispersion of (4):
the ZnO @ SiO obtained in the second step2Dispersing in a certain amount of water, and dispersing at high speed with homogenizing emulsifier to obtain uniformly dispersed dispersion, i.e. pigment ZnO @ SiO2The dispersion of (1);
step four, preparing and coating the ink-jet coating liquid:
(1) taking 20 parts of 8wt% PVA solution and 20 parts of pigment ZnO @ SiO in parts by weight2Mixing 80 parts of the dispersion, 3 parts of boric acid and 8 parts of ethanol, and dispersing at a high speed for 40min under a homogenizing emulsifying machine to obtain uniformly dispersed ink-jet coating liquid;
(2) and (3) taking the PET film with a clean surface, coating the ink-jet coating liquid by using a coating machine, and then drying in an oven at 80 ℃ to obtain the PET film with the ink-jet coating.
This example is for commercial SiO2(A-200) nanoparticles and pigment ZnO @ SiO prepared in this example2The nanoparticles were subjected to BET test comparison. The results shown in FIG. 1 show that the specific surface areas of the two nanoparticles are 221.38 m respectively2G and 265.81 m2Per g, it can be seen that the ZnO @ SiO prepared in this example2The porosity of the nano particles is far greater than that of commercial SiO2(A-200) nanoparticles, which greatly increases the ink absorption of the coating prepared in this example, making it better applicable in inkjet printing. In order to explore ZnO @ SiO2Photodegradation effect of nanoparticles, this example for ZnO Quantum dots and ZnO @ SiO2The nanoparticles were subjected to degradation tests, with rhodamine B as the staining agent, illuminated under 365nm ultraviolet light, sampled every 5min and analyzed for ultraviolet absorption, and the results obtained are shown in fig. 2. From FIG. 2, it is apparent that ZnO @ SiO2Light of nanoparticlesThe catalytic degradation effect is greatly reduced, so that the nano particles as pigments avoid the phenomenon of ink jet effect reduction caused by illumination in the ultraviolet-resistant ink jet coating, and have wide application in the aspect of ultraviolet-resistant ink jet coatings.
In this example, a pure PET film, a PVA coating coated on a PET film (PVA/PET) and ZnO @ SiO added2PVA coating of nanoparticles on PET film (ZnO @ SiO)2PVA/PET) was subjected to UV transmission analysis. As can be seen from FIG. 3, the pure PET film and PVA coating layer have no shielding effect on the ultraviolet rays in the UV-A (320 nm-400 nm) wave band, and ZnO @ SiO is added2The shielding effect of the PVA coating of the nano particles on UV-A ultraviolet rays is greatly enhanced, so that the coating has great advantages in the aspect of food packaging films; and the inset shows a printed image with high transparency and pattern definition.
Claims (7)
1. A preparation method of a nano material for improving the ultraviolet performance of an ink-jet coating of PET food packaging is characterized by comprising the following steps:
step one, coating zinc oxide ZnO @ SiO with silicon dioxide2The preparation of (1):
(1) adding tetraethoxysilane into the stirring quantum dot zinc oxide solution according to the molar ratio of Zn atoms to Si atoms of 1:1 ~ 3, and then adding water into the stirring quantum dot zinc oxide solution according to the molar ratio of tetraethoxysilane to water of 1:4 ~ 8;
(2) stirring for 24 ~ 30h until a precipitate is generated;
(3) carrying out centrifugal washing treatment on the product, collecting the product, and carrying out freeze drying;
step two, pigment ZnO @ SiO2Preparation of the dispersion of (4):
the ZnO @ SiO obtained in the step one2Dispersing in water, and performing high-speed dispersion treatment on the water by using a homogenizing emulsifying machine to obtain uniformly dispersed dispersion liquid;
step three, preparing and coating the ink-jet coating liquid:
(1) taking 10 ~ 30 parts of PVA solution and 10 parts of pigment Zn according to parts by massO@SiO270 ~ 90 parts of the dispersion liquid, 1 ~ 5 parts of boric acid and 5 ~ 10 parts of ethanol are mixed and dispersed at high speed under a homogenizing and emulsifying machine to obtain an evenly dispersed ink-jet coating liquid;
(2) and (3) taking the PET film with a clean surface, coating the ink-jet coating liquid by using a coating machine, and drying to obtain the PET film with the ink-jet coating.
2. The preparation method of the nano material for improving the ultraviolet performance of the ink-jet coating of the PET food packaging according to claim 1, characterized in that the preparation method of the quantum dot zinc oxide solution is as follows:
(1) dissolving anhydrous zinc acetate: taking 1 mol of Zn (Ac)2Dispersing the mixture into 30 ~ 50mL of absolute ethyl alcohol, gradually heating to 75 ~ 80 ℃, and dispersing and dissolving for 2 ~ 3 h;
(2) dissolving sodium hydroxide, namely taking 1 ~ 3 mol of NaOH, dispersing the NaOH in 10 ~ 30mL of absolute ethyl alcohol, and carrying out ultrasonic treatment for 10 ~ 20min until the NaOH is dissolved;
(3) reacting Zn (Ac) in the step (1)2And (3) mixing the solution with the NaOH solution in the step (2) according to the molar ratio of 1:1 ~ 3, placing the mixture at room temperature for stirring, and reacting for 1.5 ~ 3 h.
3. The preparation method of the nano material for improving the ultraviolet performance of the ink-jet coating of the PET food packaging according to claim 2, wherein the ultrasonic power is 480W, and the ultrasonic time is 10 ~ 20 min.
4. The method for preparing nano material for improving the ultraviolet performance of the ink-jet coating of the PET food package according to claim 1, wherein the rotation speed of the centrifugal washing is 9000 ~ 10000rmp/min, the times are 3 ~ 4 times, and each time is 10 min.
5. The method for preparing nano material for improving the ultraviolet performance of the ink-jet coating of the PET food packaging according to claim 1, wherein the mass concentration of the PVA solution is 2 ~ 20%.
6. The method for preparing nano material for improving the ultraviolet performance of the ink-jet coating of the PET food packaging according to claim 1, wherein the high-speed dispersion time is 40 ~ 50 min.
7. The method for preparing nano material for improving the ultraviolet performance of the ink-jet coating of the PET food packaging according to claim 1, wherein the drying temperature is 75 ~ 90 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117799259A (en) * | 2023-12-29 | 2024-04-02 | 惠州市贝斯特膜业有限公司 | PU protective film and manufacturing and application method thereof |
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| CN103436111A (en) * | 2013-07-29 | 2013-12-11 | 复旦大学 | Preparation method of water-based ultraviolet barrier coating based on ZnO quantum dots |
| CN104946037A (en) * | 2015-07-16 | 2015-09-30 | 天津科技大学 | Coating liquid for preparing uvioresistant polyester film and preparation method thereof |
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Patent Citations (4)
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| CN101967299A (en) * | 2010-09-29 | 2011-02-09 | 北京化工大学 | High-transparency ultraviolet-blocking energy-saving film and solution-fusion preparation method thereof |
| CN101974245A (en) * | 2010-09-29 | 2011-02-16 | 北京化工大学 | High-transparent ultraviolet-blocking energy-saving membrane and preparation method thereof by way of phase transfer in solution |
| CN103436111A (en) * | 2013-07-29 | 2013-12-11 | 复旦大学 | Preparation method of water-based ultraviolet barrier coating based on ZnO quantum dots |
| CN104946037A (en) * | 2015-07-16 | 2015-09-30 | 天津科技大学 | Coating liquid for preparing uvioresistant polyester film and preparation method thereof |
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| CN117799259A (en) * | 2023-12-29 | 2024-04-02 | 惠州市贝斯特膜业有限公司 | PU protective film and manufacturing and application method thereof |
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Application publication date: 20200110 |