CN107033288B - Antioxidant emulsion and antioxidant water-based coating gloss oil prepared by using same - Google Patents
Antioxidant emulsion and antioxidant water-based coating gloss oil prepared by using same Download PDFInfo
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- CN107033288B CN107033288B CN201611037189.7A CN201611037189A CN107033288B CN 107033288 B CN107033288 B CN 107033288B CN 201611037189 A CN201611037189 A CN 201611037189A CN 107033288 B CN107033288 B CN 107033288B
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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
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
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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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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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
- C08F4/00—Polymerisation catalysts
- C08F4/28—Oxygen or compounds releasing free oxygen
- C08F4/30—Inorganic compounds
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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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/12—Coatings without pigments applied as a solution using water as the only solvent, e.g. in the presence of acid or alkaline compounds
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/38—Corrosion-inhibiting agents or anti-oxidants
Abstract
The invention relates to the technical field of coating gloss oil, in particular to an antioxidant emulsion and antioxidant water-based coating gloss oil prepared by applying the antioxidant emulsion. The antioxidant emulsion is prepared from the following raw materials in percentage by weight: 30-50% of neutral pH acrylic resin solution, 29-41% of mixed monomer, 0.5-1% of emulsifier, 0.3-0.8% of initiator, 0.01-0.05% of oxidant, 0.01-0.05% of reducing agent and 10-25% of deionized water, wherein the sum of the mass percentages of the raw materials is 100%. The antioxidant emulsion can reduce possible acid and alkaline substances, reduce the probability of oxidation, and achieve the effect of gold stamping and difficult oxidation; the antioxidant aqueous coating gloss oil prepared by the antioxidant emulsion does not contain organic solvent, has low/no VOCs, is environment-friendly, nontoxic and antioxidant, and is suitable for glazing the surfaces of substrates which are easy to be subjected to gold stamping and oxidation, such as black paperboard, black paper dyeing, black paper coating and the like.
Description
Technical Field
The invention relates to the technical field of coating gloss oil, in particular to an antioxidant emulsion and antioxidant water-based coating gloss oil prepared by applying the antioxidant emulsion.
Background
The gilding paper (also called gilding foil) has the characteristics of gold, silver and color, the gold stamping is called gilding, and the silver stamping is called gilding, and is generally called gilding. The gilding paper has special metallic luster, brings bright colors to hot stamping, improves the grade of products, has fashionable appearance, and is widely applied to the packaging field, such as cosmetic packaging boxes, gift jewel boxes, high-grade shoe boxes and the like.
Gold stamping is a process of transferring a pattern on gold stamping paper on a substrate in a thermal transfer mode through proper temperature and pressure. Generally, firstly, water-based ink is printed on paper materials in a coating mode, then different patterns are thermoprinted according to requirements, and finally the paper materials are adhered into a packaging box through hot melt adhesive. However, in reality, the hot stamped patterns often turn black locally and lose metallic luster during or after subsequent processing, and particularly, the phenomenon that black coated paper has hot stamping oxidation has the highest frequency. The gilding paper is commonly called as electrochemical aluminum, has very active chemical property and is easy to oxidize when meeting acid and alkali substances. The existing water-based ink system is basically an alkaline system, when the ink is subjected to a high-temperature and high-humidity environment after being printed on paper, alkaline substances possibly remaining in the ink can cause electrochemical aluminum to be oxidized and generate spots when the alkaline substances are dissociated into a gold stamping layer, and the spots are more serious when the ink is placed for a longer time.
This spotting phenomenon can be achieved by applying a varnish layer to the surface of the paper to reduce or prevent oxidation. However, the conventional aqueous coating gloss oil is alkaline, and gold stamping is performed after coating and drying, so that alkaline substances which may corrode alumite exist inevitably, and the performance of the aqueous gloss oil is poor.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the antioxidant emulsion which can reduce possible acid and alkaline substances, reduce the probability of oxidation, achieve the effect of gold stamping and difficult oxidation and play a good protection role.
The invention also aims to provide a preparation method of the antioxidant emulsion, which is simple and convenient to operate, environment-friendly and pollution-free, and can keep the reaction rate balance in the early and later stages of the preparation process and improve the conversion rate and stability of the reaction by strictly controlling the addition amount, the addition time, the reaction temperature and the reaction time of all raw materials, so that the prepared antioxidant emulsion reduces possible acid and alkali substances, reduces the probability of oxidation, and achieves the effect of hard oxidation in gold stamping.
The invention also aims to provide antioxidant water-based coating gloss oil prepared by using the antioxidant emulsion, which belongs to a neutral pH value system, does not contain organic solvent, has low/no VOCs, is environment-friendly, nontoxic and antioxidant, is suitable for polishing the surfaces of substrates which are easy to be subjected to gold stamping and oxidation, such as black paperboard, black dyed paper, coated black paper and the like, and can achieve the effect of gold stamping and difficult oxidation.
The purpose of the invention is realized by the following technical scheme: an antioxidant emulsion is prepared from the following raw materials in percentage by weight:
neutral pH acrylic resin solution 30-50%
29-41 percent of mixed monomer
0.5 to 1 percent of emulsifier
0.3 to 0.8 percent of initiator
0.01 to 0.05 percent of oxidant
0.01 to 0.05 percent of reducing agent
10-25% of deionized water;
the sum of the mass percentages of the raw materials is 100 percent.
The raw materials are adopted to prepare the antioxidant emulsion, and the weight percentage of each raw material is strictly controlled, so that possible acid and alkali substances can be reduced, the probability of oxidation is reduced, the effect of gold stamping and difficult oxidation can be achieved, and a good protection effect can be achieved.
Preferably, the mixed monomer is prepared by mixing styrene, butyl acrylate, isooctyl acrylate and hydroxyethyl methacrylate in a weight ratio of 6-10: 3-5: 20-25: 0.5-1. The invention adopts the mixture of styrene, butyl acrylate, isooctyl acrylate and hydroxyethyl methacrylate as a mixed monomer, and strictly controls the weight ratio of the mixed monomer to be 6-10: 3-5: 20-25: 0.5-1, can effectively improve the stability, adhesive force and wet friction performance of the antioxidant emulsion, so that the coating gloss oil has more optimized comprehensive performance.
Preferably, the emulsifier is alkyl polyoxyethylene ether phosphate, the initiator is ammonium persulfate, the oxidant is tert-butyl hydroperoxide, and the reducing agent is a gripper block.
The invention adopts alkyl polyoxyethylene ether phosphate as the emulsifier, has excellent emulsibility, wettability, dispersibility and permeability, and can improve the adhesive force, weather resistance and water resistance of the antioxidant emulsion; by adopting ammonium persulfate as an initiator, the initiation rate is high, no impurity ions are introduced to cause side reaction, and the stability and the water resistance of the antioxidant emulsion can be improved; by adopting tert-butyl hydroperoxide as an oxidant, the method has the advantages of good oxidability, high selectivity, reusability and the like, is safe to use and easy to control, and can improve the emulsion polymerization effect and the thermal stability of the antioxidant emulsion; the gripper block is used as a reducing agent and reacts with the oxidant tert-butyl hydroperoxide to generate free radicals, so that the reaction of residual monomers is more sufficient, and the purposes of full utilization and reaction of raw materials are achieved.
Preferably, the pH value of the neutral pH acrylic resin solution is 7.0-8.0, the solid content is 30-35%, the acid value is 200-250mg KOH/g, the Tg value is 90-120 ℃, and the relative molecular weight is 8000-15000. The neutral pH acrylic resin solution with the characteristics is non-toxic, pollution-free and high in stability, and can be used as a protective colloid for preparing an antioxidant emulsion.
The other purpose of the invention is realized by the following technical scheme: the preparation method of the antioxidant emulsion comprises the following steps:
(1) adding the neutral pH acrylic resin solution into a reaction device, and heating to 75-85 ℃;
(2) adding an initiator into deionized water for mixing to prepare an initiator solution with the mass concentration of 5-15%; mixing the mixed monomer, the emulsifier and the deionized water, and dispersing at a high speed to prepare a pre-emulsion;
(3) dripping 35-45% of the initiator solution prepared in the step (2) into a reaction device according to the volume total amount at the temperature of 80-85 ℃, dripping 3-7% of the pre-emulsion prepared in the step (2) into the reaction device according to the volume total amount, and then preserving heat for 15-25min at the temperature of 80-85 ℃;
(4) dropwise adding the residual initiator solution and the pre-emulsion obtained after dropwise adding in the step (3) into a reaction device at the same time, and then preserving heat for 0.8-1.2h at the temperature of 80-85 ℃ to obtain a first reaction solution;
(5) cooling the first reaction liquid obtained in the step (4) to 72-78 ℃, adding an oxidant, then adding a reducing agent, and keeping the temperature at 72-78 ℃ for reaction for 10-20min to obtain a second reaction liquid;
(6) and (5) cooling the second reaction liquid obtained in the step (5) to prepare the antioxidant emulsion.
By adopting the steps for preparing the antioxidant emulsion and strictly controlling the reaction temperature and the reaction time, the invention can effectively reduce possible acid and alkaline substances in the prepared antioxidant emulsion, reduce the probability of oxidation and ensure that the bronzed paper has excellent antioxidant performance; in addition, the initiator and the pre-emulsifier are added in batches and the rest amount is added simultaneously, so that the change of the reaction process can be reduced, the reaction rate before and after the reaction is balanced, the conversion rate and the stability of the reaction can be improved, and the quality of the antioxidant emulsion is improved.
Preferably, in the step (2), the adding amount of the deionized water is 25-35% of the adding amount of the mixed monomer, the high-speed dispersion time after mixing is 8-12min, and the dispersion rotation speed is 800-1000 r/min. The invention can improve the performances of the pre-emulsion such as dispersibility, stability and the like by strictly controlling the addition of the deionized water for preparing the pre-emulsion and the high-speed dispersion time and dispersion speed after mixing, and is beneficial to balancing the reaction process and reaction rate of the subsequent preparation of the antioxidant emulsion.
Preferably, in the step (3), the dropping time of the initiator solution is 2-8min, and the dropping time of the pre-emulsion is 8-12 min; in the step (4), the dropping time of the initiator solution is 4-4.5h, and the dropping time of the pre-emulsion is 3.5-4.5 h; in the step (5), the adding time of the oxidant is 8-12min, and the adding time of the reducing agent is 12-18 min. The invention can keep the reaction rate in the later period before and after the reaction balanced, ensure the reaction to be complete and complete, reduce the change of the reaction process and improve the stability of the reaction and the quality of the antioxidant emulsion by strictly controlling the adding time of the initiator solution and the pre-emulsion in batches and controlling the adding time of the oxidant and the reducing agent.
The invention also aims to realize the following technical scheme: the antioxidant water-based coating gloss oil prepared by using the antioxidant emulsion is prepared by mixing and dispersing the following raw materials in percentage by weight:
90-95% of antioxidant emulsion
1 to 5 percent of wax additive
0.2 to 0.6 percent of defoaming agent
2-5% of deionized water;
the sum of the mass percentages of the raw materials is 100 percent.
The water-based coating gloss oil prepared by the raw materials has the characteristics of low/no VOCs, environmental protection, no toxicity and the like, can achieve the effect of gold stamping and difficult oxidation, has a good protection effect, and is suitable for glazing the surfaces of substrates which are easy to gold stamping and oxidize, such as black paperboard, black dyed paper, coated black paper and the like.
Preferably, the wax assistant is an aqueous polytetrafluoroethylene modified wax dispersion. The wax auxiliary agent adopted by the invention is a water-based polytetrafluoroethylene modified wax dispersoid, WW-1077 of Krevilie is selected, the softening point of the wax dispersoid reaches 340 ℃, and the wax dispersoid has very superior scratch resistance, wear resistance and high temperature resistance and excellent water resistance and ageing resistance; by adopting the wax dispersion, the water resistance, ageing resistance, scraping resistance, wear resistance and high temperature resistance of the gloss oil can be improved, and the subsequent high-temperature gold stamping process is facilitated.
Preferably, the defoaming agent is a mixture of a silicone defoaming agent and a mineral oil defoaming agent in a weight ratio of 1: 1-2. The invention adopts the mixture of the organic silicon defoamer and the mineral oil defoamer as the defoamer, strictly controls the weight ratio of the defoamer to be 1:1-2, has strong defoaming capability and strong foam inhibition capability, and has excellent thermal stability, acid and alkali resistance, diffusivity, permeability and chemical stability.
The invention has the beneficial effects that: the antioxidant emulsion can reduce possible acid and alkaline substances, reduce the probability of oxidation, achieve the effect of gold stamping and difficult oxidation, and play a good role in protection.
The preparation method of the antioxidant emulsion is simple and convenient to operate, environment-friendly and pollution-free, and by strictly controlling the addition amount, the addition time, the reaction temperature and the reaction time of all raw materials, the reaction rate balance in the early and later stages of the preparation process can be kept, the conversion rate and the stability of the reaction can be improved, the possible acid and alkali substances are reduced in the prepared antioxidant emulsion, the probability of oxidation is reduced, and the effect that gold stamping is not easy to oxidize is achieved.
The antioxidant water-based coating gloss oil belongs to a neutral pH value system, does not contain organic solvents, has low/no VOCs, is environment-friendly, nontoxic and antioxidant, is suitable for polishing the surfaces of substrates which are easy to be gilded and oxidized, such as black paperboard, black dyed paper, coated black paper and the like, and can achieve the effect of gilding and difficult to oxidize.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
An antioxidant emulsion is prepared by taking a neutral pH acrylic resin solution Joncryl LMV 7025 as a protective colloid, taking a mixed monomer, an emulsifier, an initiator and deionized water as raw materials, and carrying out pre-emulsification, seed reaction and polymerization reaction, and is specifically prepared from the following raw materials in percentage by weight:
neutral pH acrylic resin solution (Joncryl LMV 7025) 400
Mixed monomer 356
Emulsifier 8
Initiator 6.6
Oxidizing agent 0.2
Reducing agent 0.2
Deionized water 239.
The mixed monomer is prepared from styrene, butyl acrylate, isooctyl acrylate and hydroxyethyl methacrylate in a weight ratio of 8: 4: 23: 0.7 of the composition.
The emulsifier is alkyl polyoxyethylene ether phosphate, the initiator is ammonium persulfate, the oxidant is tert-butyl hydroperoxide, and the reducing agent is a gripper block.
Preferably, the pH value of the neutral pH acrylic resin solution is 7.0-8.0, the solid content is 30-35%, the acid value is 200-250mg KOH/g, the Tg value is 90-120 ℃, and the relative molecular weight is 8000-15000.
The preparation method of the antioxidant emulsion comprises the following steps:
(1) 400kg of a neutral pH acrylic resin solution (Joncryl LMV 7025) and 46.6kg of deionized water were added to a reaction apparatus, and the temperature was raised to 80 ℃;
(2) mixing 6.6kg of ammonium persulfate and 59.4kg of deionized water to prepare an initiator solution with the mass concentration of 5%; mixing a mixed monomer (95 kg of styrene, 45kg of butyl acrylate, 210kg of isooctyl acrylate and 6kg of hydroxyethyl methacrylate), 8kg of an emulsifier and 103kg of deionized water, and dispersing at a high speed, wherein the dispersion rotating speed is 900r/min to prepare a pre-emulsion;
(3) dropwise adding 26.4kg of the initiator solution prepared in the step (2) into a reaction device at 80 ℃, dropwise adding 23kg of the pre-emulsion prepared in the step (2) into the reaction device, and then preserving heat for 15min at 80 ℃;
(4) dropwise adding the residual initiator solution and the pre-emulsion in the step (3) into a reaction device at the same time, flushing the head tank with 5kg of deionized water after dropwise adding the initiator solution, flushing the head tank with 10kg of deionized water after dropwise adding the pre-emulsion, and then preserving heat for 0.8h at 80 ℃ to obtain a first reaction solution;
(5) cooling the first reaction liquid obtained in the step (4) to 75 ℃, adding a mixed liquid of 0.2kg of oxidant and 5kg of deionized water, then adding a mixed liquid of 0.2kg of reducing agent and 10kg of deionized water, and keeping the temperature at 75 ℃ for reacting for 15min to obtain a second reaction liquid;
(6) and (4) cooling the second reaction solution obtained in the step (5) to prepare the antioxidant emulsion with the solid content of 47%, the pH value of 7.0-7.5, the viscosity of 100-.
In the step (2), the addition amount of the deionized water is 25% of the addition amount of the mixed monomer, the high-speed dispersion time after mixing is 10min, and the dispersion rotating speed is 900 r/min.
In the step (3), the dropping time of the initiator solution is 5min, and the dropping time of the pre-emulsion is 10 min; in the step (4), the dropping time of the initiator solution is 4.3 hours, and the dropping time of the pre-emulsion is 4 hours; in the step (5), the adding time of the oxidizing agent is 10min, and the adding time of the reducing agent is 15 min.
An antioxidant aqueous coating gloss oil prepared by applying the antioxidant emulsion is prepared by mixing and dispersing the following raw materials in percentage by weight:
92 percent of antioxidant emulsion
3 percent of wax additive
0.3 percent of defoaming agent
4.7 percent of deionized water.
The wax additive is water-based polytetrafluoroethylene modified wax dispersoid WW-1077.
The defoaming agent is a mixture of an organic silicon defoaming agent and a mineral oil defoaming agent in a weight ratio of 1: 2.
The water-based coating gloss oil is prepared by the following steps of adding antioxidant emulsion into a dispersing device at normal temperature, wherein the dispersing speed is 700r/min, sequentially adding a wax assistant and a defoaming agent, stirring for 15min, and adjusting the viscosity by deionized water to obtain the antioxidant water-based coating gloss oil with the pH =7.0 ~ 7.5.5 and the viscosity of 35 ~ 50 s/(coating with a 4# cup at 30 ℃).
Example 2
This embodiment differs from embodiment 1 described above in that:
an antioxidant emulsion is prepared by taking a neutral pH acrylic resin solution Joncryl LMV 7085-E as a protective colloid, taking a mixed monomer, an emulsifier, an initiator and deionized water as raw materials, and carrying out pre-emulsification, seed reaction and polymerization reaction, and is specifically prepared from the following raw materials in percentage by weight:
neutral pH acrylic resin solution (Joncryl LMV 7085-E) 400
Mixed monomer 346
Emulsifier 8
Initiator 6.6
Oxidizing agent 0.2
Reducing agent 0.2
Deionized water 249.
The preparation method of the antioxidant emulsion comprises the following steps:
(1) adding 400kg of neutral pH acrylic resin solution (Joncryl LMV 7085-E) and 46.6kg of deionized water into a reaction device, and heating to 80 ℃;
(2) mixing 6.6kg of ammonium persulfate and 59.4kg of deionized water to prepare an initiator solution with the mass concentration of 5%; mixing the mixed monomer (95 kg of styrene, 35kg of butyl acrylate, 200kg of isooctyl acrylate and 6kg of hydroxyethyl methacrylate), 8kg of emulsifier and 113kg of deionized water, and dispersing at a high speed of 800-.
(3) Dropwise adding 26.4kg of the initiator solution prepared in the step (2) into a reaction device at 80 ℃, dropwise adding 23kg of the pre-emulsion prepared in the step (2) into the reaction device, and then preserving heat for 15min at 80 ℃;
(4) dropwise adding the residual initiator solution and the pre-emulsion in the step (3) into a reaction device at the same time, flushing the head tank with 5kg of deionized water after dropwise adding the initiator solution, flushing the head tank with 10kg of deionized water after dropwise adding the pre-emulsion, and then preserving heat for 0.8h at 80 ℃ to obtain a first reaction solution;
(5) cooling the first reaction liquid obtained in the step (4) to 75 ℃, adding a mixed liquid of 0.2kg of oxidant and 5kg of deionized water, then adding a mixed liquid of 0.2kg of reducing agent and 10kg of deionized water, and keeping the temperature at 75 ℃ for reacting for 15min to obtain a second reaction liquid;
(6) and (4) cooling the second reaction solution obtained in the step (5) to prepare the antioxidant emulsion with the solid content of 47%, the pH value of 7.0-7.5, the viscosity of 100-.
An antioxidant aqueous coating gloss oil prepared by applying the antioxidant emulsion is prepared by mixing and dispersing the following raw materials in percentage by weight:
antioxidant emulsion 93%
3 percent of wax additive
0.3 percent of defoaming agent
3.7 percent of deionized water.
Comparative example 1
A common water-based coating gloss oil is prepared by mixing and dispersing the following raw materials in percentage by weight:
ordinary emulsion 92%
3 percent of wax additive
0.3 percent of defoaming agent
4.7 percent of deionized water;
the common emulsion is emulsion basf J-77.
The wax additive is a PE wax dispersion.
The defoaming agent is a mixture of an organic silicon defoaming agent and a mineral oil defoaming agent in a weight ratio of 1: 2.
The common water-based coating gloss oil is prepared by the following steps of adding common emulsion into a dispersing device at normal temperature, wherein the dispersing speed is 700r/min, sequentially adding a wax auxiliary agent and a defoaming agent, stirring for 15min, and adjusting the viscosity by deionized water to obtain the common water-based coating gloss oil with the pH =7.0 ~ 7.5.5 and the viscosity of 35 ~ 50 s/(coating with a 4# cup at 30 ℃).
Comparative example 2
A common water-based coating gloss oil is prepared by mixing and dispersing the following raw materials in percentage by weight:
ordinary emulsion 92%
3 percent of wax additive
0.3 percent of defoaming agent
4.7 percent of deionized water.
The common emulsion is prepared from emulsion BASF J-90 and emulsion BASF J-624 in a weight ratio of 32: 60, respectively.
The wax additive is a PE wax dispersion.
The defoaming agent is a mixture of an organic silicon defoaming agent and a mineral oil defoaming agent in a weight ratio of 1: 2.
The preparation method of the common water-based coating gloss oil is the same as that of comparative example 1, and the details are not repeated.
The above aqueous coating gloss oil prepared according to the above examples 1-2 and comparative examples 1-2 was prepared by scraping a layer of gloss oil on a coated paper with black ink with an RDS 12 wire bar, drying in an oven at 80 deg.C for 30min, standing at room temperature for 2h, gilding, and testing oxidation grade in a constant temperature and humidity cabinet.
The test results are expressed as follows:
| sample (I) | Clear away the light | Example 1 | Example 2 | Comparative example 1 | Comparative example 2 |
| Oxidation resistance grade | 1 | 9 | 9 | 7 | 6 |
| Durability | Difference (D) | Is excellent in | Is excellent in | Good effect | Good effect |
| High temperature resistance | Difference (D) | Is excellent in | Is excellent in | Good effect | Good effect |
| Anti-adhesion | Non-blocking | Non-blocking | Non-blocking | Non-blocking | Non-blocking |
And (3) testing conditions are as follows:
(1) oxidation resistance grade: the thermoprinting paper is placed in a breathable plastic box, the plastic box is placed in a constant temperature and humidity box, the set parameters are 50 ℃, the humidity is 90%, the current oxidation resistance grade is obtained when no oxidation spots appear in the specified time, and the test results are shown in the following table:
| grade | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| Time of day | ＜8h | ＜16h | ＜24h | ＜32h | ＜40h | ＜48h | ＜56h | ＜64h | ＜72h |
(2) Durability: the thermoprinting paper is placed in a laboratory (the temperature is 25 ℃, the humidity is 50%), whether oxidation spots appear or not is observed after 15 days, and if the oxidation spots do not appear, the durability is good.
(3) High temperature resistance: and (3) thermoprinting the gold stamping material on the surface of the printing water-based ink paper product at the temperature of 200 ℃, and placing the paper product in an environment with the temperature of 25 ℃ and the humidity of 40% for 24 hours. The high-temperature resistance is excellent when no black spots appear, and the high-temperature resistance is poor when black spots appear.
(4) Anti-adhesion: the coated sample was folded in half face to face, and tested for 30 minutes at 40 ℃ with a Specac back adhesion tester at 0.2 ton, and the sample was taken out to see whether or not adhesion occurred.
According to the test results, compared with the common water-based coating gloss oil prepared by using the common emulsion in the comparative examples 1-2, the anti-oxidation water-based coating gloss oil prepared by the invention has the advantages that the patterns of black card paper, black dyed paper and the like subjected to gold stamping after being polished are excellent in anti-oxidation performance, high-temperature hot stamping resistance is realized, no oxidation is caused after long-term placement, the service cycle of the gold stamping patterns of the packaging printed products is greatly prolonged, and the anti-oxidation effect is remarkable and improved in performance.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (4)
1. An antioxidant aqueous coating gloss oil, which is characterized in that: the material is prepared by mixing and dispersing the following raw materials in percentage by weight:
the sum of the mass percentages of the raw materials is 100 percent;
the wax auxiliary agent is a water-based polytetrafluoroethylene modified wax dispersoid;
the defoaming agent is a mixture of an organic silicon defoaming agent and a mineral oil defoaming agent in a weight ratio of 1: 1-2;
the antioxidant emulsion is prepared from the following raw materials in percentage by weight:
the sum of the mass percentages of the raw materials is 100 percent;
the pH value of the neutral pH acrylic resin solution is 7.0-8.0, the solid content is 30-35%, the acid value is 200-120 mg KOH/g, the Tg value is 90-120 ℃, and the relative molecular weight is 8000-15000;
the mixed monomer is prepared from styrene, butyl acrylate, isooctyl acrylate and hydroxyethyl methacrylate according to the weight ratio of 6-10: 3-5: 20-25: 0.5-1;
the emulsifier is alkyl polyoxyethylene ether phosphate, the initiator is ammonium persulfate, the oxidant is tert-butyl hydroperoxide, and the reducing agent is a gripper block.
2. The antioxidant aqueous coating varnish of claim 1, wherein: the preparation method of the antioxidant emulsion comprises the following steps:
(1) adding the neutral pH acrylic resin solution into a reaction device, and heating to 75-85 ℃;
(2) adding an initiator into deionized water for mixing to prepare an initiator solution with the mass concentration of 5-15%; mixing the mixed monomer, the emulsifier and the deionized water, and dispersing at a high speed to prepare a pre-emulsion;
(3) dripping 35-45% of the initiator solution prepared in the step (2) into a reaction device according to the volume total amount at the temperature of 80-85 ℃, dripping 3-7% of the pre-emulsion prepared in the step (2) into the reaction device according to the volume total amount, and then preserving heat for 15-25min at the temperature of 80-85 ℃;
(4) dropwise adding the residual initiator solution and the pre-emulsion obtained after dropwise adding in the step (3) into a reaction device at the same time, and then preserving heat for 0.8-1.2h at the temperature of 80-85 ℃ to obtain a first reaction solution;
(5) cooling the first reaction liquid obtained in the step (4) to 72-78 ℃, adding an oxidant, then adding a reducing agent, and keeping the temperature at 72-78 ℃ for reaction for 10-20min to obtain a second reaction liquid;
(6) and (5) cooling the second reaction liquid obtained in the step (5) to prepare the antioxidant emulsion.
3. The antioxidant aqueous coating varnish of claim 2, wherein: in the step (2), the adding amount of the deionized water is 25-35% of the adding amount of the mixed monomer, the high-speed dispersion time after mixing is 8-12min, and the dispersion rotating speed is 800-.
4. The antioxidant aqueous coating varnish of claim 2, wherein: in the step (3), the dropping time of the initiator solution is 2-8min, and the dropping time of the pre-emulsion is 8-12 min; in the step (4), the dropping time of the initiator solution is 4-4.5h, and the dropping time of the pre-emulsion is 3.5-4.5 h; in the step (5), the adding time of the oxidant is 8-12min, and the adding time of the reducing agent is 12-18 min.
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| CN110379293B (en) * | 2019-07-18 | 2021-10-26 | 广东天元实业集团股份有限公司 | Bottom blue-developing heat-sensitive label and preparation method thereof |
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