CN109852134A - A kind of preparation method of aqueous metal ink - Google Patents
A kind of preparation method of aqueous metal ink Download PDFInfo
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- CN109852134A CN109852134A CN201910029273.1A CN201910029273A CN109852134A CN 109852134 A CN109852134 A CN 109852134A CN 201910029273 A CN201910029273 A CN 201910029273A CN 109852134 A CN109852134 A CN 109852134A
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Abstract
The present invention relates to ink preparation technical fields, and in particular to a kind of preparation method of aqueous metal ink.The present invention using Mian Jiang liquid as raw material obtain hydro-thermal coke, by polyurethane, copper sulphate, the substances such as hydro-thermal coke and sodium tartrate are scattered in deionized water, obtain chemical bronze plating liquid, finally iron powder is put into chemical bronze plating liquid, sediment is put into hydrogen and restores drying, obtain metallic pigments, the present invention aoxidizes hydro-thermal coke in the chemical bronze plating liquid of high-temperature heating, polymethyl acrylate can increase the copper facing area of iron powder, it is not likely to produce bubbling, metallic pigments are the iron powder of copper metal cladding in the present invention, play the protective effect to copper powder, organic coating can inhibit the growth that copper crystal grain is precipitated, keep the accumulation of copper coating more fine and close, it is improved copper coating to the corrosion resistance and oxygen-proof property of inorganic acid highly basic, finally oxidative impurities are driven away, it is fixed in printing layer, it has broad application prospects.
Description
Technical field
The present invention relates to ink preparation technical fields, and in particular to a kind of preparation method of aqueous metal ink.
Background technique
It is well known that ink is largely industrially to depend on metal base table by way of printing spraying at present
Face.Metal ink refers to replaces the pigments or dyes in traditional ink to be formulated with tiny sheet metal, main component
It include: main body gloss oil, metal powder material, colored ink.Metal ink is the ink with unique metal luminous effect.Metal ink
Pigment be mainly bronze and silver powder (copper powder and aluminium powder), other pigment of people can also be added to generate the ink with particular color,
Referred to as coloring metal ink.Metal ink has glittering metallic luster, is mainly used in packing and decorating printing, prints to beautification
Brush product, raising added value of product have immeasurable effect.With the continuous progress of technology, the functionality of product and appearance and
Feature of environmental protection requirement is also higher and higher, can effectively solve that ink does not lose metal effect again in the problems such as environmental protection, conduction, color, will
The key subjects that must be tackled key problems in industry must be become.
But contain petroleum solvent in metal ink, and it is equivalent to the over-head distillate and light diesel fuel last runnings of aviation kerosine, it is this
Contain more polycyclic aromatic hydrocarbons in petroleum solvent, residual quantity is big on printed matter, and duration is long, either to children
Or adult can cause body harm, this is also the environomental pollution source in Printing ink producing and use process.Existing part enterprise
Part petroleum solvent was substituted with soybean oil already, soybean oil is not only environmentally friendly but also is renewable resource, is favored by people.But it will be big
When metal ink is made in soya-bean oil, it often will appear metallic pigments (such as Cu-Zn alloy powder) and change colour because of corrosion dimmed problem, to influence
The high gloss of ink and the performances such as water-fast, chemical-resistant resistance and electrical isolation.
In view of the above-mentioned problems, water-based ink can not only reduce printed matter surface due to not containing volatile organic solvent
VOC is remained to improve production environment in workshop, can also farthest reduce the destruction to periphery ecological environment, and use
When water-based ink, printing equipment cleaning is more convenient.Therefore, water-based ink has good as a kind of printing material of green
Application prospect.If China Patent No. is 201510467805.1, patent name is " a kind of environmentally protective printing ink of aqua type ",
The invention provides a kind of environmentally protective printing ink of aqua type, is prepared from the following raw materials: acrylic resin, colorant, disappears at solvent
Infusion, dispersing agent, wax.Compared with prior art, this ink is the water-based inks using water as solvent to the invention, without containing waving
Hair property organic solvent, will not understand that health causes damages to Workers Producing Printing Ink and printing worker.Meanwhile water-based inks have compared with
Good stability, it is nonflammable, cost is reduced, and corrosiveness is not present to printing plate, meets modern environmentally protective theory.But
There are the characteristics that the shortcomings that following aspect in practical applications: (1) due to metallic pigments, itself performance-is vivaciously easily oxidized
Dimmed, blackening and lose metallic luster, especially in alkaline water-based system, metallic pigments are easier to aoxidize blackening agglomeration so that
Aqueous metal ink is restricted in the application；(2) the package processing technique of water-based metal pigment is not mature enough, and metallic pigments are not
It can be wrapped up well, then being easily oxidized；(3) compared with same kind of products at abroad, there is stability poor, Yi Chen
It forms sediment, is easy to change, a series of not disadvantages such as alkali resistant, not anti-ethyl alcohol, non-water resistant, dry slow, low in glossiness, quality is always not as good as import
Similar product.
Therefore, how in the case where not influencing metal-like, while main body ink solid content can also be taken into account and guarantee ink
Adhesive force, material property itself is stable and environmental protection is this field important technological problems to be solved.
Summary of the invention
Present invention mainly solves the technical issues of, for metallic pigments in aqueous metal ink, on the one hand performance itself is relatively living
It sprinkles, is easily oxidized dimmed, blackening and loses metallic luster, another aspect metallic pigments technique for packing is not mature enough, metallic pigments
The defect that exposure is eventually oxidized for a long time, provides a kind of preparation method of aqueous metal ink.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of aqueous metal ink, it is characterised in that: the aqueous metal ink is by self-control metallic pigments, aqueous
Solvent, molecular weight are 15000~20000D aqueous polyurethane, antioxidant, wetting dispersing agent, surfactant composition.
The specific preparation step of the aqueous metal ink are as follows:
20~25 parts of self-control metallic pigments are mixed to get with 200~220 parts of aqueous solvents in a stirring kettle and mix disperse materials, with
It is 15000~20000D aqueous polyurethane, 8~12 parts of antioxidants, 8~10 parts of wetting and dispersings that 40~50 parts of molecular weight are added afterwards
Agent, 10~15 parts of surfactants, are dispersed with stirring with the rotating speed cutting of 1500~2000r/min in shear mixer, are obtained
Aqueous metal ink.
The specific preparation step of the self-control metallic pigments are as follows:
(1) 200~250mL cotton pulp black liquor is put into the reaction kettle with air valve, reaction kettle is sealed, with 40~50mL/min's
Ventilation Rate is passed through carbon dioxide gas into reaction kettle by air valve, and ventilation continues 10~15min, closes breather valve, heating
200~220 DEG C are warming up to, 7~8h of insulation reaction obtains reaction mass；
(2) above-mentioned reaction mass is mixed with quick lime, is heated to 80~90 DEG C, clear up 4~5min, obtain the causticity slurry that disappears
Liquid, the causticity that will disappear slurries are separated by filtration, and collect filter residue, filter residue are put into the baking oven that set temperature is 100~110 DEG C, and dry 4
~10h obtains hydro-thermal coke；
(3) 100~120g copper powder is taken to be placed in a beaker, it is molten to pour into the sulfuric acid that 200~300mL mass fraction is 35% along walls of beaker
Liquid, heat temperature raising are stirred continuously until copper powder dissolution is begun with then to the concentrated ammonia liquor that mass fraction is 25% is added in beaker
Precipitating generates, and persistently plus ammonium hydroxide is completely dissolved until precipitating, and obtains copper ammon solution；
(4) copper ammon solution, hydro-thermal coke, glyoxalic acid, sodium tartrate, polymethyl acrylate and sodium carbonate are put into deionized water
Dispersion is mixed 20~25min, obtains chemical bronze plating liquid；
(5) 400~500mL chemical bronze plating liquid is put into beaker, is heated to 90~100 DEG C, into beaker launch 40~
50g reduced iron powder, 40~50min of insulation reaction are separated by filtration to obtain sediment, and putting the precipitate in set temperature is 70~80
DEG C baking oven in, be put into ammonolysis craft hydrogen furnace after dry 2~3h, heat temperature raising, continue to restore dry 40~50min, ventilation
Charcoal ash are blown away, self-control metallic pigments are obtained.
The aqueous solvent is one of ethylene glycol, propylene glycol, butyl glycol ether.
The antioxidant is monoalkoxy Pyrophosphate Type Yitanate Coupling Agent, chelating titanate coupling agent, single alkane
One of oxygroup type titante coupling agent.
The wetting dispersing agent is one of Sodium Polyacrylate or polyethylene glycol.
The surfactant is polyoxyethylene carboxylate, neopelex, alkyl diphenyl ether disulphonic acid
One of sodium.
Cotton pulp black liquor solid masses content is 25% in the specific preparation step (1) of the self-control metallic pigments.
Reaction mass and quick lime mixing mass ratio are 10 ︰ in the specific preparation step (2) of the self-control metallic pigments
1。
Temperature is preferably 60~65 when sulfuric acid dissolution copper powder in the specific preparation step (3) of the self-control metallic pigments
℃。
The each component raw material of chemical bronze plating liquid is in parts by weight in the specific preparation step (4) of the described self-control metallic pigments
Preferably 40~50 parts of copper ammon solutions, 20~30 parts of hydro-thermal coke, 15~20 parts of glyoxalic acids, 60~70 parts of sodium tartrates, 20~
25 parts of polymethyl acrylate and 20~25 parts of sodium carbonate, 400~500 parts of deionized waters.
Reduction drying temperature is 150 in ammonolysis craft hydrogen furnace in the specific preparation step (5) of the self-control metallic pigments
~200 DEG C.
The beneficial effects of the present invention are:
(1) present invention by Mian Jiang ?liquid be put into reaction kettle, be passed through heating and thermal insulation after carbon dioxide gas and react, obtain reactant
Reaction mass quick lime is cleared up causticity, is separated by filtration rear re-dry and obtains hydro-thermal coke, by polyurethane, copper sulphate, water by material
The substances such as hot coke and sodium tartrate are scattered in deionized water, obtain chemical bronze plating liquid, finally disposably throw reduced iron powder
Enter in the chemical bronze plating liquid of heating, insulation reaction obtains sediment, will be put into ammonolysis craft hydrogen and continues also after drying precipitate
Original is dry, obtains metallic pigments, the raw material that the present invention utilizes is cathode copper waste liquid, circuit board spent etching solution etc., if by these
Waste liquid direct emission is not only stained significantly environment, also results in significant wastage, is free of strong acid and strong base etc. in chemical bronze plating liquid
The noxious materials such as corrosive substance and formaldehyde, thus metallic pigments end of the invention is safe and environmentally friendly, in addition by hydro-thermal coke
It is aoxidized in the chemical bronze plating liquid of high-temperature heating, is reacted with water and generate reducibility gas-carbonoxide and hydrogen, chemically copper plating bath
In the reducibility gas that slowly releases copper ion oxidation is precipitated on iron powder surface, oxidizing gas avoidable in this way is attached to
Iron powder surface makes it keep elemental stage in the preparation process of metallic pigments, in addition polymethyl acrylate having as iron powder
Machine coating can increase the copper facing area of iron powder, make to contact tightness degree promotion in copper-coated iron composite powder end between copper and iron, be not easy
Generate bubbling；
(2) iron powder that metallic pigments coat in the present invention for copper metal, the copper metal of outer surface have coloring function, internal iron powder
There is protective effect to copper, because iron is more active than copper, the primary battery formed between the two, iron is that cathode is first oxidized, to play
Protective effect to copper powder, and the iron oxide formed after iron oxidation is similar with same color, is all red, will not make metallic pigments
Discoloration, furthermore chemical bronze plating liquid polymethyl acrylate under higher temperatures environment can inhibit the life that copper crystal grain is precipitated as organic coating
It is long, cause the speed of growth of crystal grain to be less than the formation speed of nucleus, forms more tiny copper metal crystal grain, make the heap of copper coating
Product is more fine and close, and copper coating surface is not likely to produce protrusion, and the crystal grain of gained metal copper coating is more and tiny, and organic coating can be right
The hole of copper coating is filled package, is improved copper coating to the corrosion resistance and oxygen-proof property of inorganic acid highly basic,
Reducing agent used in iron powder copper coating is mainly iron itself and hydro-thermal coke, in addition also contains a small amount of glyoxalic acid and hypophosphorous acid
Ammonium, both substances can restore copper ion, and the binding force of organic coating and the coat of metal can also be made to increase, finally with ammonia point
Solution hydrogen furnace oxidative impurities are driven away, aqueous metal ink solidify after can in conjunction with the titanate coupling agent of anti-oxidation effect,
It is fixed in printing layer, has broad application prospects.
Specific embodiment
The cotton pulp black liquor that 200~250mL solid masses content is 25% is put into the reaction kettle with air valve, sealing is anti-
Kettle to be answered, with the Ventilation Rate of 40~50mL/min, carbon dioxide gas is passed through into reaction kettle by air valve, ventilation continues 10~
15min closes breather valve, is heated to 200~220 DEG C, 7~8h of insulation reaction obtains reaction mass；By above-mentioned reactant
Material is that 10 ︰ 1 are mixed with quick lime in mass ratio, is heated to 80~90 DEG C, clears up 4~5min, obtains the causticity slurries that disappear, will
The causticity that disappears slurries are separated by filtration, and collect filter residue, filter residue are put into the baking oven that set temperature is 100~110 DEG C, dry 4~
10h obtains hydro-thermal coke；100~120g copper powder is taken to be placed in a beaker, pouring into 200~300mL mass fraction along walls of beaker is
35% sulfuric acid solution is heated to 60~65 DEG C, is stirred continuously until copper powder dissolves, then to addition quality point in beaker
The concentrated ammonia liquor for being 25% is counted, precipitating is begun with and generates, persistently plus ammonium hydroxide is completely dissolved until precipitating, and obtains copper ammon solution；By weight
Number meter, by 40~50 parts of copper ammon solutions, 20~30 parts of hydro-thermal coke, 15~20 parts of glyoxalic acids, 60~70 parts of sodium tartrates, 20
~25 parts of polymethyl acrylate and 20~25 parts of sodium carbonate, which are put into 400~500 parts of deionized waters, to be dispersed, and mixing 20~
25min obtains chemical bronze plating liquid；400~500mL chemical bronze plating liquid is put into beaker, is heated to 90~100 DEG C, to
40~50g reduced iron powder is launched in beaker, 40~50min of insulation reaction is separated by filtration to obtain sediment, puts the precipitate in and set
Determine in the baking oven that temperature is 70~80 DEG C, be put into ammonolysis craft hydrogen furnace after dry 2~3h, be heated to 150~200 DEG C,
Continue to restore dry 40~50min, charcoal ash are blown away in ventilation, obtain self-control metallic pigments；According to parts by weight, in a stirring kettle will
20~25 parts of above-mentioned self-control metallic pigments are mixed to get with 200~220 parts of aqueous solvents mixes disperse materials, is then added 40~50
Part molecular weight is 15000~20000D aqueous polyurethane, 8~12 parts of antioxidants, 8~10 parts of wetting dispersing agents, 10~15 parts
Surfactant is dispersed with stirring in shear mixer with the rotating speed cutting of 1500~2000r/min, obtains water-based metal oil
Ink, the aqueous solvent are one of ethylene glycol, propylene glycol, butyl glycol ether, and the antioxidant is that monoalkoxy is burnt
One of phosphate type titanate coupling agent, chelating titanate coupling agent, monoalkoxy type titante coupling agent or its
Combination, the wetting dispersing agent are one of Sodium Polyacrylate or polyethylene glycol, and the surfactant is fatty acid
One of polyoxyethylene ester, neopelex, alkyl diphenyl ether disulphonic acid sodium or combinations thereof.
Aqueous solvent: ethylene glycol antioxidant: monoalkoxy Pyrophosphate Type Yitanate Coupling Agent wetting dispersing agent: poly- third
Olefin(e) acid natrium surfactant: polyoxyethylene carboxylate reaction mass the preparation method comprises the following steps: being by 200mL solid masses content
25% cotton pulp black liquor is put into the reaction kettle with air valve, is sealed reaction kettle with the Ventilation Rate of 40mL/min and is passed through air valve
It is passed through carbon dioxide gas into reaction kettle, ventilates and continues 10min, closes breather valve, is heated to 200 DEG C, insulation reaction
7h obtains reaction mass.
Hydro-thermal coke the preparation method comprises the following steps: with quick lime being in mass ratio that 10 ︰ 1 are mixed by above-mentioned reaction mass, heating rises
Temperature clears up 4min, obtains the causticity slurries that disappear to 80 DEG C, and the causticity that will disappear slurries are separated by filtration, and collects filter residue, filter residue is put into setting
In the baking oven that temperature is 100 DEG C, dry 4h obtains hydro-thermal coke.
Copper ammon solution the preparation method comprises the following steps: 100g copper powder is taken to be placed in a beaker, pouring into 200mL mass fraction along walls of beaker is
35% sulfuric acid solution is heated to 60 DEG C, is stirred continuously until copper powder dissolution, is then to mass fraction is added in beaker
25% concentrated ammonia liquor begins with precipitating and generates, and persistently plus ammonium hydroxide is completely dissolved until precipitating, and obtains copper ammon solution.
Chemical bronze plating liquid the preparation method comprises the following steps: according to parts by weight, by 40 parts of copper ammon solutions, 20 parts of hydro-thermal coke, 15 parts
Glyoxalic acid, 60 parts of sodium tartrates, 20 parts of polymethyl acrylate and 20 parts of sodium carbonate, which are put into 400 parts of deionized waters, to be dispersed, mixing
20min is stirred, chemical bronze plating liquid is obtained.
Self-control metallic pigments the preparation method comprises the following steps: 400mL chemical bronze plating liquid is put into beaker, be heated to 90 DEG C,
40g reduced iron powder is launched into beaker, insulation reaction 40min is separated by filtration to obtain sediment, puts the precipitate in set temperature
To be put into ammonolysis craft hydrogen furnace after dry 2h, being heated to 150 DEG C, continue to restore dry 40min in 70 DEG C of baking ovens,
Charcoal ash are blown away in ventilation, obtain self-control metallic pigments.
Aqueous metal ink the preparation method comprises the following steps: according to parts by weight, in a stirring kettle by 20 parts of above-mentioned self-control metal face
Material is mixed to get with 200 parts of ethylene glycol mixes disperse materials, and it is 15000D aqueous polyurethane, 8 parts of lists that 40 parts of molecular weight, which are then added,
Alkoxy Pyrophosphate Type Yitanate Coupling Agent, 8 parts of Sodium Polyacrylates, 10 parts of polyoxyethylene carboxylates, in shear mixer
In be dispersed with stirring with the rotating speed cutting of 1500r/min, obtain aqueous metal ink.
Aqueous solvent: propylene glycol antioxidant: chelating titanate coupling agent wetting dispersing agent: Sodium Polyacrylate surface is living
Property agent: neopelex reaction mass the preparation method comprises the following steps: by 225mL solid masses content be 25% cotton pulp black liquor
It is put into the reaction kettle with air valve, sealing reaction kettle is passed through by air valve into reaction kettle with the Ventilation Rate of 45mL/min
Carbon dioxide gas ventilates and continues 13min, closes breather valve, is heated to 210 DEG C, insulation reaction 7h obtains reactant
Material.
Hydro-thermal coke the preparation method comprises the following steps: with quick lime being in mass ratio that 10 ︰ 1 are mixed by above-mentioned reaction mass, heating rises
Temperature clears up 4min, obtains the causticity slurries that disappear to 85 DEG C, and the causticity that will disappear slurries are separated by filtration, and collects filter residue, filter residue is put into setting
In the baking oven that temperature is 105 DEG C, dry 7h obtains hydro-thermal coke.
Copper ammon solution the preparation method comprises the following steps: 110g copper powder is taken to be placed in a beaker, pouring into 250mL mass fraction along walls of beaker is
35% sulfuric acid solution is heated to 63 DEG C, is stirred continuously until copper powder dissolution, is then to mass fraction is added in beaker
25% concentrated ammonia liquor begins with precipitating and generates, and persistently plus ammonium hydroxide is completely dissolved until precipitating, and obtains copper ammon solution.
Chemical bronze plating liquid the preparation method comprises the following steps: according to parts by weight, by 45 parts of copper ammon solutions, 25 parts of hydro-thermal coke, 17 parts
Glyoxalic acid, 65 parts of sodium tartrates, 23 parts of polymethyl acrylate and 23 parts of sodium carbonate, which are put into 450 parts of deionized waters, to be dispersed, mixing
23min is stirred, chemical bronze plating liquid is obtained.
Self-control metallic pigments the preparation method comprises the following steps: 450mL chemical bronze plating liquid is put into beaker, be heated to 95 DEG C,
45g reduced iron powder is launched into beaker, insulation reaction 45min is separated by filtration to obtain sediment, puts the precipitate in set temperature
To be put into ammonolysis craft hydrogen furnace after dry 2h, being heated to 175 DEG C, continue to restore dry 45min in 75 DEG C of baking ovens,
Charcoal ash are blown away in ventilation, obtain self-control metallic pigments.
Aqueous metal ink the preparation method comprises the following steps: according to parts by weight, in a stirring kettle by 23 parts of above-mentioned self-control metal face
Material obtains mixing disperse materials with 210 parts of mixed with propylene glycol, and it is 17500D aqueous polyurethane, 10 portions of chelas that 45 parts of molecular weight, which are then added,
Mould assembly titanate coupling agent, 9 parts of Sodium Polyacrylates, 13 parts of neopelexes, with 1750r/min in shear mixer
Rotating speed cutting be dispersed with stirring, obtain aqueous metal ink.
Aqueous solvent: butyl glycol ether antioxidant: monoalkoxy type titante coupling agent wetting dispersing agent: poly- second two
Alcohol
Surfactant: alkyl diphenyl ether disulphonic acid sodium reaction mass the preparation method comprises the following steps: being by 250mL solid masses content
25% cotton pulp black liquor is put into the reaction kettle with air valve, is sealed reaction kettle with the Ventilation Rate of 50mL/min and is passed through air valve
It is passed through carbon dioxide gas into reaction kettle, ventilates and continues 15min, closes breather valve, is heated to 220 DEG C, insulation reaction
8h obtains reaction mass.
Hydro-thermal coke the preparation method comprises the following steps: with quick lime being in mass ratio that 10 ︰ 1 are mixed by above-mentioned reaction mass, heating rises
Temperature clears up 5min, obtains the causticity slurries that disappear to 90 DEG C, and the causticity that will disappear slurries are separated by filtration, and collects filter residue, filter residue is put into setting
In the baking oven that temperature is 110 DEG C, dry 10h obtains hydro-thermal coke.
Copper ammon solution the preparation method comprises the following steps: 120g copper powder is taken to be placed in a beaker, pouring into 300mL mass fraction along walls of beaker is
35% sulfuric acid solution is heated to 65 DEG C, is stirred continuously until copper powder dissolution, is then to mass fraction is added in beaker
25% concentrated ammonia liquor begins with precipitating and generates, and persistently plus ammonium hydroxide is completely dissolved until precipitating, and obtains copper ammon solution.
Chemical bronze plating liquid the preparation method comprises the following steps: according to parts by weight, by 50 parts of copper ammon solutions, 30 parts of hydro-thermal coke, 20 parts
Glyoxalic acid, 70 parts of sodium tartrates, 25 parts of polymethyl acrylate and 25 parts of sodium carbonate, which are put into 500 parts of deionized waters, to be dispersed, mixing
25min is stirred, chemical bronze plating liquid is obtained.
Self-control metallic pigments the preparation method comprises the following steps: 500mL chemical bronze plating liquid is put into beaker, be heated to 100 DEG C,
50g reduced iron powder is launched into beaker, insulation reaction 50min is separated by filtration to obtain sediment, puts the precipitate in set temperature
To be put into ammonolysis craft hydrogen furnace after dry 3h, being heated to 200 DEG C, continue to restore dry 50min in 80 DEG C of baking ovens,
Charcoal ash are blown away in ventilation, obtain self-control metallic pigments.
Aqueous metal ink the preparation method comprises the following steps: according to parts by weight, in a stirring kettle by 25 parts of above-mentioned self-control metal face
Material is mixed to get with 220 parts of butyl glycol ethers mixes disperse materials, and it is 20000D aqueous polyurethane, 12 that 50 parts of molecular weight, which are then added,
Part monoalkoxy type titante coupling agent, 10 parts of polyethylene glycol, 15 parts of alkyl diphenyl ether disulphonic acid sodium, in shear mixer
It is dispersed with stirring with the rotating speed cutting of 2000r/min, obtains aqueous metal ink.
Comparative example 1: it is essentially identical with the preparation method of example 1, it has only the difference is that antioxidant is not added.
Comparative example 2: it is essentially identical with the preparation method of example 2, it has only the difference is that wetting dispersing agent is not added.
Comparative example 3: the aqueous metal ink of Zhaoqing company production.
Aqueous metal ink in aqueous metal ink produced by the present invention and comparative example is detected, testing result is such as
Shown in table 1:
Water resistance test
It is detected using instrument, using the aqueous metal ink of Examples 1 to 3 prepared by the present invention and comparative example 1~3 as sample
Product are brushed (glass plate is first waxed) on a glass several times, quiet to put 7d with a thickness of 1.5mm, be then placed in baking oven 50 DEG C ±
2 DEG C are dried for 24 hours, and 3h is placed after taking-up, do waterproof experiment, and impermeability 0.3MPa, keeping 30min ne-leakage is qualification, is protected
Hold 45min ne-leakage be it is good, keep 60min ne-leakage be it is excellent.
The aqueous metal ink of Examples 1 to 3 prepared by the present invention and comparative example 1~3 is made in high temperature and humidity resistance test
It for sample, is placed in that temperature is 60 DEG C, humidity is to stand 240h in the environment of 90%RH, measures performance.
Inoxidizability is tested using the aqueous metal ink of Examples 1 to 3 prepared by the present invention and comparative example 1~3 as sample
Product place 500h in artificial sunshine weather analogy machine, measure performance.
1 performance measurement result of table
From the data in table 1, it can be seen that aqueous metal ink tinting strength, tinting power produced by the present invention is good, printing is bright in colour, glossiness is high, attachment
Power is strong, layer of ink is not fallen off, and non-toxic and tasteless, safety and environmental protection, indices reach similar products at home and abroad advanced level, product matter
It measures, suits large area to popularize and use, there is wide prospect of the application.
Claims (10)
1. a kind of preparation method of aqueous metal ink, it is characterised in that specific preparation step are as follows: in a stirring kettle by 20~25
Part self-control metallic pigments are mixed to get with 200~220 parts of aqueous solvents mixes disperse materials, and 40~50 parts of molecular weight, which are then added, is
15000~20000D aqueous polyurethane, 8~12 parts of antioxidants, 8~10 parts of wetting dispersing agents, 10~15 parts of surfactants,
It is dispersed with stirring in shear mixer with the rotating speed cutting of 1500~2000r/min, obtains aqueous metal ink；
The specific preparation step of the self-control metallic pigments are as follows:
(1) 200~250mL cotton pulp black liquor is put into the reaction kettle with air valve, reaction kettle is sealed, with 40~50mL/min
Ventilation Rate, carbon dioxide gas is passed through into reaction kettle by air valve, ventilation continues 10~15min, closes breather valve, adds
Heat is warming up to 200~220 DEG C, and 7~8h of insulation reaction obtains reaction mass；
(2) above-mentioned reaction mass is mixed with quick lime, is heated to 80~90 DEG C, clear up 4~5min, obtain the causticity slurry that disappears
Liquid, the causticity that will disappear slurries are separated by filtration, and collect filter residue, filter residue are put into the baking oven that set temperature is 100~110 DEG C, and dry 4
~10h obtains hydro-thermal coke；
(3) 100~120g copper powder is taken to be placed in a beaker, it is molten to pour into the sulfuric acid that 200~300mL mass fraction is 35% along walls of beaker
Liquid, heat temperature raising are stirred continuously until copper powder dissolution is begun with then to the concentrated ammonia liquor that mass fraction is 25% is added in beaker
Precipitating generates, and persistently plus ammonium hydroxide is completely dissolved until precipitating, and obtains copper ammon solution；
(4) copper ammon solution, hydro-thermal coke, glyoxalic acid, sodium tartrate, polymethyl acrylate and sodium carbonate are put into deionized water
Middle dispersion is mixed 20~25min, obtains chemical bronze plating liquid；
(5) 400~500mL chemical bronze plating liquid is put into beaker, is heated to 90~100 DEG C, into beaker launch 40~
50g reduced iron powder, 40~50min of insulation reaction are separated by filtration to obtain sediment, and putting the precipitate in set temperature is 70~80
DEG C baking oven in, be put into ammonolysis craft hydrogen furnace after dry 2~3h, heat temperature raising, continue to restore dry 40~50min, ventilation
Charcoal ash are blown away, self-control metallic pigments are obtained.
2. a kind of preparation method of aqueous metal ink according to claim 1, it is characterised in that: the aqueous solvent
For one of ethylene glycol, propylene glycol, butyl glycol ether.
3. a kind of preparation method of aqueous metal ink according to claim 1, it is characterised in that: the antioxidant is
Monoalkoxy Pyrophosphate Type Yitanate Coupling Agent, chelating titanate coupling agent, in monoalkoxy type titante coupling agent
One kind.
4. a kind of preparation method of aqueous metal ink according to claim 1, it is characterised in that: the wetting and dispersing
Agent is one of Sodium Polyacrylate or polyethylene glycol.
5. a kind of preparation method of aqueous metal ink according to claim 1, it is characterised in that: the surface-active
Agent is one of polyoxyethylene carboxylate, neopelex, alkyl diphenyl ether disulphonic acid sodium.
6. a kind of preparation method of aqueous metal ink according to claim 1, it is characterised in that: the self-control metal
Cotton pulp black liquor solid masses content is 25% in the specific preparation step (1) of pigment.
7. a kind of preparation method of aqueous metal ink according to claim 1, it is characterised in that: the self-control metal
Reaction mass and quick lime mixing mass ratio are 10 ︰ 1 in the specific preparation step (2) of pigment.
8. a kind of preparation method of aqueous metal ink according to claim 1, it is characterised in that: the self-control metal
Temperature is preferably 60~65 DEG C when sulfuric acid dissolution copper powder in the specific preparation step (3) of pigment.
9. a kind of preparation method of aqueous metal ink according to claim 1, it is characterised in that: the self-control metal
The each component raw material of chemical bronze plating liquid is preferably that 40~50 parts of cuprammoniums are molten in parts by weight in the specific preparation step (4) of pigment
Liquid, 20~30 parts of hydro-thermal coke, 15~20 parts of glyoxalic acids, 60~70 parts of sodium tartrates, 20~25 parts of polymethyl acrylate and 20
~25 parts of sodium carbonate, 400~500 parts of deionized waters.
10. a kind of preparation method of aqueous metal ink according to claim 1, it is characterised in that: the self-control gold
Reduction drying temperature is 150~200 DEG C in ammonolysis craft hydrogen furnace in the specific preparation step (5) of category pigment.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093781A (en) * | 2011-01-27 | 2011-06-15 | 广东天龙油墨集团股份有限公司 | Aqueous metal ink and preparation method thereof |
| CN105562713A (en) * | 2016-01-30 | 2016-05-11 | 常州市君成机械有限公司 | Preparing method for copper coated iron composite powder |
| CN108193196A (en) * | 2017-12-29 | 2018-06-22 | 唐林元 | A kind of preparation method of environmental friendly, anti-corrosive erosion chemical bronze plating liquid |
| CN108311692A (en) * | 2018-05-03 | 2018-07-24 | 佛山九陌科技信息咨询有限公司 | A kind of preparation method at anti-oxidant copper-coated iron composite powder end |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093781A (en) * | 2011-01-27 | 2011-06-15 | 广东天龙油墨集团股份有限公司 | Aqueous metal ink and preparation method thereof |
| CN105562713A (en) * | 2016-01-30 | 2016-05-11 | 常州市君成机械有限公司 | Preparing method for copper coated iron composite powder |
| CN108193196A (en) * | 2017-12-29 | 2018-06-22 | 唐林元 | A kind of preparation method of environmental friendly, anti-corrosive erosion chemical bronze plating liquid |
| CN108311692A (en) * | 2018-05-03 | 2018-07-24 | 佛山九陌科技信息咨询有限公司 | A kind of preparation method at anti-oxidant copper-coated iron composite powder end |
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Application publication date: 20190607 |