CN110028842A - A kind of wear-resisting ink of noctilucence and preparation method thereof - Google Patents
A kind of wear-resisting ink of noctilucence and preparation method thereof Download PDFInfo
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- CN110028842A CN110028842A CN201910262492.4A CN201910262492A CN110028842A CN 110028842 A CN110028842 A CN 110028842A CN 201910262492 A CN201910262492 A CN 201910262492A CN 110028842 A CN110028842 A CN 110028842A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/46—Polyesters chemically modified by esterification
- C08G63/48—Polyesters chemically modified by esterification by unsaturated higher fatty oils or their acids; by resin acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/91—Polymers modified by chemical after-treatment
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
- C09D11/104—Polyesters
- C09D11/105—Alkyd resins
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- 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
- C09D11/50—Sympathetic, colour changing or similar inks
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Abstract
The present invention discloses a kind of wear-resisting ink of noctilucence, is made of following raw material: 35-50 parts of modified alkyd resins, 35-45 parts of phosphorescent pigments, 35-50 parts of polyurethane, 8-15 parts of photoinitiators, 5-12 parts of defoaming agents, 55-70 parts of dehydrated alcohols, 15-25 parts of nano silicas；The invention also discloses a kind of preparation methods of the wear-resisting ink of noctilucence；The present invention is during the preparation process using modified alkyd resin, polyurethane, phosphorescent pigment and nano silica as raw material; using dehydrated alcohol as solvent under conditions of nitrogen makees protection gas; a kind of wear-resisting ink of noctilucence is prepared by process means such as ultrasonic disperses; wear-resisting property can be further increased by the way that nano silica is added; the ink not only has excellent permanent noctilucence time and good wear-resisting property; and stability with higher; it can satisfy multiple product demand, use scope is wider.
Description
Technical field
The invention belongs to Printing ink producing technical field, specially a kind of wear-resisting ink of noctilucence and preparation method thereof.
Background technique
The manufacture of ink is a complicated chemical engineering, its material relates to organic polymer synthesis and oxidation also
Original, diazotising, displacement reaction, the chemical changes such as complex reaction.Meanwhile being related to mechanics, optics, chromatism, surface chemistry etc.
Subject.Currently, more and more products begin to use luminous ink, be mainly used for means of transportation, military installations, public place of entertainment,
Public place, emergency indicating system, billboard etc., facilitate daily life to a certain extent.But now
Luminous ink on the market, by the test of profession, the duration of noctilucent function is insufficient, and wear-resisting property is inadequate, Wu Fageng
Mostly widely applied.
Chinese invention patent CN107057464A discloses a kind of environment-friendly long-life luminous ink and preparation method thereof, the environmental protection
It include the aqueous polyurethane of 50-80 parts by weight, the ester alcohol solvent of 80-100 parts by weight, 30-50 weight in long-acting noctilucent ink
Measure the modified luminescent powder of the silicon fluoride of number, the Lauxite of 5-10 parts by weight, the bamboo charcoal of 3-8 parts by weight, 3-7 parts by weight
Several pigment, the wax of 4-6 parts by weight, the montmorillonite of 2-7 parts by weight, 1-3 parts by weight surfactant.In the present invention
It only needs to absorb various visible lights, including indoor light using environment-friendly long-life luminous ink made from above-mentioned raw materials, so that it may
Dark place or night realize continuous illumination, and the sunset glow time that shines is long, luminous intensity it is high and, shine uniform.In addition silicon fluoride is modified
Dispersibility, storage stability of the luminescent powder in ink, it is with good economic efficiency.But the noctilucence oil of invention preparation
Black purposes is relatively narrow, and drying time is longer and adhesive property is not excellent enough.
Summary of the invention
In order to overcome above-mentioned technical problem, the present invention provides a kind of wear-resisting ink of noctilucence and preparation method thereof.With modification
Alkyd resin, polyurethane, phosphorescent pigment and nano silica are as raw material, with anhydrous second under conditions of nitrogen makees protection gas
Alcohol prepares a kind of wear-resisting ink of noctilucence as solvent, by process means such as ultrasonic disperses, by the way that nano silica is added
Wear-resisting property can be further increased, which not only has excellent permanent noctilucence time and good wear-resisting property, but also
Stability with higher can satisfy multiple product demand, which only needs of short duration absorption visible light can be black
It is in the dark permanent to shine, and fluorescent lifetime is long, and luminous intensity is high and more uniform, and the ink itself has good wearability
Energy and stability, can more be widely used in multiple fields.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of wear-resisting ink of noctilucence, is made of following raw material: 35-50 parts of modified alkyd resins, 35-45 parts of noctilucence
Pigment, 35-50 parts of polyurethane, 8-15 parts of photoinitiators, 5-12 parts of defoaming agents, 55-70 parts of dehydrated alcohols, 15-25 parts of nanometers two
Silica；
The wear-resisting ink of the noctilucence is made by the following method:
Step S1, modified alkyd resin, polyurethane and half dehydrated alcohol are added in three-necked flask, are heated to 80 DEG C,
Nitrogen discharge air is passed through after heat preservation 1h, control mixing speed is 85r/min, stirs 30min, is warming up to 95 DEG C, keep the temperature 1h, makees
A liquid is spare；
Step S2, phosphorescent pigment and the other half dehydrated alcohol are added in beaker, 45 DEG C of heating water baths at the uniform velocity stir
Photoinitiator is added after 15min, is warming up to 75 DEG C, with the revolving speed magnetic agitation 30min of 180r/min, makees B liquid；
Step S3, A liquid is poured into B liquid, at the uniform velocity stirring 5min, defoaming agent is added, passes through high speed after ultrasonic disperse 30min
Blender is stirred, and the revolving speed for controlling blender is 9000r/min, is transferred in vacuum oven dry 2h after stirring 1h,
Control vacuum degree is -0.09MPa, and temperature is 85 DEG C；
Step S4, addition nano silica is poured into after mixing carries out ball milling in ball mill, control turning for ball mill
Speed is 2000r/min, and the wear-resisting ink of noctilucence that partial size is 8-13 μm is made.
Further, the modified alkyd resin is made of following raw material: 5-8 parts of benzoic acid, 3-5 parts of sub- oil
Acid, 5-10 parts of glutaric anhydrides, 50-75 parts of dimethylbenzene, 10-20 parts of dimethylethanolamines, 3-8 parts of sodium peroxydisulfates.
Further, the modified alkyd resin is made by the following method:
(1) benzoic acid, linoleic acid, glutaric anhydride and phthalic anhydride are added in the three-necked flask equipped with dimethylbenzene,
50 DEG C of heating water baths simultaneously at the uniform velocity stir 20min, and dimethylethanolamine is added, is warming up to 75 DEG C, at the uniform velocity stirring 5min；
(2) it is transferred in the vacuum reaction kettle that vacuum degree is -0.10MPa, is warming up to 150 DEG C and keeps the temperature 2h, observing response
Kettle water yield is heated up when water yield is stablized with the speed of 5 DEG C/h, until 250 DEG C, it is kept the temperature, is examined at this temperature
Degree of esterification is surveyed, is cooled down after being 18mgKOH/g when the acid value of detection, until being down to 30 DEG C, vacuum pumps the diformazan of reflux
Alkyd resin is made in benzene；
(3) alkyd resin is transferred in beaker and is heated to 150 DEG C, addition lauric acid, with the revolving speed magnetic of 200r/min
Power stirs 30min, keeps the temperature 45min at this temperature, and half sodium peroxydisulfate is added, the other half sodium peroxydisulfate is added after keeping the temperature 1h,
30min is kept the temperature, n-butanol is added up to 60 DEG C in cooling, and modified alkyd resin, control alkyd resin, lauric acid and positive fourth is made
The weight ratio of alcohol is 1: 3: 5.
The present invention prepares alkyd resin by benzoic acid, linoleic acid, glutaric anhydride, phthalic anhydride, and alkyd resin is not
Only there is hydroxyl, carboxyl, double bond and ester group, the also very strong main chain of polarized and nonpolar side chain, alkyd resin can be assigned
Good glossiness and flexibility, and the wetability of alkyd resin and adhesion property are preferable, but weatherability, corrosion resistance and
Water resistance is not able to satisfy the needs of actual production but, and the ester bond easy fracture in alkyd resin, will lead to and passes through alkyd resin
Resin layering can even occur for the ink performance decline of preparation, and ink is caused not to be available, so needing to carry out alkyd resin
It is modified.
Due to having hydroxyl, carboxyl, double bond and ester group on alkyd resin, it is easy to react with acid, so passing through laurel
Acid is modified alkyd resin, and with the hydroxyl of alkyd resin polycondensation reaction can occur for lauric carboxyl, passes through to be formed later
Hydrogen bond lauric acid is grafted on alkyd resin molecule, reduce the interfacial tension between lauric acid and acrylic resin, energy
Enough enhance alkyd resin stability and weatherability, further enhance the wear-resisting ink of noctilucence of preparation stability and
Weather resistance.
Further, the phosphorescent pigment is made of following raw material: 15-28 parts of polyacetylene, 35-45 parts of aniline,
3-8 parts of cadmium yellows, 35-50 parts of glycerine, 3-8 parts of lauryl sodium sulfate, 8-15 parts of ethyl orthosilicates, 3-8 parts of barium sulfate, 5-8
Part luminescent powder.
Further, the phosphorescent pigment is made by the following method:
(1) polyacetylene is added in the beaker equipped with half glycerine, is passed through nitrogen to completely cut off air, 60 DEG C of heating water baths
Lauryl sodium sulfate is added in 30min, carries out high speed centrifugation with the revolving speed of 10000r/min after 70 DEG C of heating water bath 5h, will sink
Starch washes of absolute alcohol is clean, is put into 80 DEG C of drying boxes dry 2h, obtains mixture；
(2) ethyl orthosilicate is added in the other half glycerine, 25% ammonium hydroxide is added, triethanolamine is added dropwise after 10min, it is even
Until solution is clarified, the weight ratio of control ethyl orthosilicate, 25% ammonium hydroxide and triethanolamine is 5: 0.3: 0.1 for speed stirring；
(3) mixture for obtaining step (1) is added in the solution of step (2), after magnetic agitation 1h, is transferred to crucible
In, aniline, luminescent powder, cadmium yellow and barium sulfate are sequentially added, is warming up to 280 DEG C, heats 5h at this temperature, is taken out, is stood cold
But it grinds, sieves with 100 mesh sieve after 1h, phosphorescent pigment is made.
Further, the photoinitiator is one of benzoin dimethylether, benzoin ethyl ether and benzoin isopropyl ether
Or it is several.
Further, the defoaming agent is one of benzyl carbinol oleate, tributyl phosphate and dimethicone or several
Kind.
A kind of preparation method of the wear-resisting ink of noctilucence, includes the following steps:
Step S1, modified alkyd resin, polyurethane and half dehydrated alcohol are added in three-necked flask, are heated to 80 DEG C,
Nitrogen discharge air is passed through after heat preservation 1h, control mixing speed is 85r/min, stirs 30min, is warming up to 95 DEG C, keep the temperature 1h, makees
A liquid is spare；
Step S2, phosphorescent pigment and the other half dehydrated alcohol are added in beaker, 45 DEG C of heating water baths at the uniform velocity stir
Photoinitiator is added after 15min, is warming up to 75 DEG C, with the revolving speed magnetic agitation 30min of 180r/min, makees B liquid；
Step S3, A liquid is poured into B liquid, at the uniform velocity stirring 5min, defoaming agent is added, passes through high speed after ultrasonic disperse 30min
Blender is stirred, and the revolving speed for controlling blender is 9000r/min, is transferred in vacuum oven dry 2h after stirring 1h,
Control vacuum degree is -0.09MPa, and temperature is 85 DEG C；
Step S4, addition nano silica is poured into after mixing carries out ball milling in ball mill, control turning for ball mill
Speed is 2000r/min, and the wear-resisting ink of noctilucence that partial size is 8-13 μm is made.
Beneficial effects of the present invention:
(1) present invention with modified alkyd resin, polyurethane, phosphorescent pigment and receives during preparing noctilucence wear-resisting ink
Rice silica, using dehydrated alcohol as solvent under conditions of nitrogen makees protection gas, passes through the works such as ultrasonic disperse as raw material
Skill means prepare a kind of wear-resisting ink of noctilucence, can further increase wear-resisting property by the way that nano silica is added, the oil
Ink not only has excellent permanent noctilucence time and good wear-resisting property, but also stability with higher, can satisfy more
Kind product demand, use scope are wider；
(2) present invention is prepared for a kind of phosphorescent pigment during preparing noctilucence wear-resisting ink, by with polyacetylene, benzene
Amine, cadmium yellow etc. are used as raw material, a kind of phosphorescent pigment are prepared using lauryl sodium sulfate as ionic surfactant, which passes through
Short time, which absorbs luminous energy, to be issued energy in the form of visible light in dark condition, so assigning the ink finally prepared
Good permanent luminous effect；
(3) the wear-resisting ink of noctilucence prepared by the present invention only needs of short duration absorption visible light that can send out for a long time in the dark
Light, and fluorescent lifetime is long, and luminous intensity is high and more uniform, and the ink itself has good wear-resisting property and stabilization
Property, it can more be widely used in multiple fields.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, all other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of wear-resisting ink of noctilucence, is made of following raw material: 35 parts of modified alkyd resins, 35 parts of phosphorescent pigments,
35 parts of polyurethane, 8 parts of benzoin ethyl ethers, 5 parts of dimethicones, 55 parts of dehydrated alcohols, 15 parts of nano silicas；
The wear-resisting ink of the noctilucence is made by the following method:
Step S1, modified alkyd resin, polyurethane and half dehydrated alcohol are added in three-necked flask, are heated to 80 DEG C,
Nitrogen discharge air is passed through after heat preservation 1h, control mixing speed is 85r/min, stirs 30min, is warming up to 95 DEG C, keep the temperature 1h, makees
A liquid is spare；
Step S2, phosphorescent pigment and the other half dehydrated alcohol are added in beaker, 45 DEG C of heating water baths at the uniform velocity stir
Benzoin ethyl ether is added after 15min, is warming up to 75 DEG C, with the revolving speed magnetic agitation 30min of 180r/min, makees B liquid；
Step S3, A liquid is poured into B liquid, at the uniform velocity stirring 5min, dimethicone is added, passes through after ultrasonic disperse 30min
High-speed mixer is stirred, and the revolving speed for controlling blender is 9000r/min, is transferred to drying in vacuum oven after stirring 1h
2h, control vacuum degree are -0.09MPa, and temperature is 85 DEG C；
Step S4, addition nano silica is poured into after mixing carries out ball milling in ball mill, control turning for ball mill
Speed is 2000r/min, and the wear-resisting ink of noctilucence that partial size is 8-13 μm is made；
The modified alkyd resin is made by the following method:
(1) benzoic acid, linoleic acid, glutaric anhydride and phthalic anhydride are added in the three-necked flask equipped with dimethylbenzene,
50 DEG C of heating water baths simultaneously at the uniform velocity stir 20min, and dimethylethanolamine is added, is warming up to 75 DEG C, at the uniform velocity stirring 5min；
(2) it is transferred in the vacuum reaction kettle that vacuum degree is -0.10MPa, is warming up to 150 DEG C and keeps the temperature 2h, observing response
Kettle water yield is heated up when water yield is stablized with the speed of 5 DEG C/h, until 250 DEG C, it is kept the temperature, is examined at this temperature
Degree of esterification is surveyed, is cooled down after being 18mgKOH/g when the acid value of detection, until being down to 30 DEG C, vacuum pumps the diformazan of reflux
Alkyd resin is made in benzene；
(3) alkyd resin is transferred in beaker and is heated to 150 DEG C, addition lauric acid, with the revolving speed magnetic of 200r/min
Power stirs 30min, keeps the temperature 45min at this temperature, and half sodium peroxydisulfate is added, the other half sodium peroxydisulfate is added after keeping the temperature 1h,
30min is kept the temperature, n-butanol is added up to 60 DEG C in cooling, and modified alkyd resin, control alkyd resin, lauric acid and positive fourth is made
The weight ratio of alcohol is 1: 3: 5；
The phosphorescent pigment is made by the following method:
(1) polyacetylene is added in the beaker equipped with half glycerine, is passed through nitrogen to completely cut off air, 60 DEG C of heating water baths
Lauryl sodium sulfate is added in 30min, carries out high speed centrifugation with the revolving speed of 10000r/min after 70 DEG C of heating water bath 5h, will sink
Starch washes of absolute alcohol is clean, is put into 80 DEG C of drying boxes dry 2h, obtains mixture；
(2) ethyl orthosilicate is added in the other half glycerine, 25% ammonium hydroxide is added, triethanolamine is added dropwise after 10min, it is even
Until solution is clarified, the weight ratio of control ethyl orthosilicate, 25% ammonium hydroxide and triethanolamine is 5: 0.3: 0.1 for speed stirring；
(3) mixture for obtaining step (1) is added in the solution of step (2), after magnetic agitation 1h, is transferred to crucible
In, aniline, luminescent powder, cadmium yellow and barium sulfate are sequentially added, is warming up to 280 DEG C, heats 5h at this temperature, is taken out, is stood cold
But it grinds, sieves with 100 mesh sieve after 1h, phosphorescent pigment is made.
Embodiment 2
A kind of wear-resisting ink of noctilucence, is made of following raw material: 40 parts of modified alkyd resins, 38 parts of phosphorescent pigments,
40 parts of polyurethane, 10 parts of benzoin ethyl ethers, 8 parts of dimethicones, 60 parts of dehydrated alcohols, 18 parts of nano silicas；
The wear-resisting ink of the noctilucence is made by the following method:
Step S1, modified alkyd resin, polyurethane and half dehydrated alcohol are added in three-necked flask, are heated to 80 DEG C,
Nitrogen discharge air is passed through after heat preservation 1h, control mixing speed is 85r/min, stirs 30min, is warming up to 95 DEG C, keep the temperature 1h, makees
A liquid is spare；
Step S2, phosphorescent pigment and the other half dehydrated alcohol are added in beaker, 45 DEG C of heating water baths at the uniform velocity stir
Benzoin ethyl ether is added after 15min, is warming up to 75 DEG C, with the revolving speed magnetic agitation 30min of 180r/min, makees B liquid；
Step S3, A liquid is poured into B liquid, at the uniform velocity stirring 5min, dimethicone is added, passes through after ultrasonic disperse 30min
High-speed mixer is stirred, and the revolving speed for controlling blender is 9000r/min, is transferred to drying in vacuum oven after stirring 1h
2h, control vacuum degree are -0.09MPa, and temperature is 85 DEG C；
Step S4, addition nano silica is poured into after mixing carries out ball milling in ball mill, control turning for ball mill
Speed is 2000r/min, and the wear-resisting ink of noctilucence that partial size is 8-13 μm is made.
Embodiment 3
A kind of wear-resisting ink of noctilucence, is made of following raw material: 45 parts of modified alkyd resins, 40 parts of phosphorescent pigments,
45 parts of polyurethane, 12 parts of benzoin ethyl ethers, 10 parts of dimethicones, 65 parts of dehydrated alcohols, 20 parts of nano silicas；
The wear-resisting ink of the noctilucence is made by the following method:
Step S1, modified alkyd resin, polyurethane and half dehydrated alcohol are added in three-necked flask, are heated to 80 DEG C,
Nitrogen discharge air is passed through after heat preservation 1h, control mixing speed is 85r/min, stirs 30min, is warming up to 95 DEG C, keep the temperature 1h, makees
A liquid is spare；
Step S2, phosphorescent pigment and the other half dehydrated alcohol are added in beaker, 45 DEG C of heating water baths at the uniform velocity stir
Benzoin ethyl ether is added after 15min, is warming up to 75 DEG C, with the revolving speed magnetic agitation 30min of 180r/min, makees B liquid；
Step S3, A liquid is poured into B liquid, at the uniform velocity stirring 5min, dimethicone is added, passes through after ultrasonic disperse 30min
High-speed mixer is stirred, and the revolving speed for controlling blender is 9000r/min, is transferred to drying in vacuum oven after stirring 1h
2h, control vacuum degree are -0.09MPa, and temperature is 85 DEG C；
Step S4, addition nano silica is poured into after mixing carries out ball milling in ball mill, control turning for ball mill
Speed is 2000r/min, and the wear-resisting ink of noctilucence that partial size is 8-13 μm is made.
Embodiment 4
A kind of wear-resisting ink of noctilucence, is made of following raw material: 50 parts of modified alkyd resins, 45 parts of phosphorescent pigments,
50 parts of polyurethane, 15 parts of benzoin ethyl ethers, 12 parts of dimethicones, 70 parts of dehydrated alcohols, 25 parts of nano silicas；
The wear-resisting ink of the noctilucence is made by the following method:
Step S1, modified alkyd resin, polyurethane and half dehydrated alcohol are added in three-necked flask, are heated to 80 DEG C,
Nitrogen discharge air is passed through after heat preservation 1h, control mixing speed is 85r/min, stirs 30min, is warming up to 95 DEG C, keep the temperature 1h, makees
A liquid is spare；
Step S2, phosphorescent pigment and the other half dehydrated alcohol are added in beaker, 45 DEG C of heating water baths at the uniform velocity stir
Benzoin ethyl ether is added after 15min, is warming up to 75 DEG C, with the revolving speed magnetic agitation 30min of 180r/min, makees B liquid；
Step S3, A liquid is poured into B liquid, at the uniform velocity stirring 5min, dimethicone is added, passes through after ultrasonic disperse 30min
High-speed mixer is stirred, and the revolving speed for controlling blender is 9000r/min, is transferred to drying in vacuum oven after stirring 1h
2h, control vacuum degree are -0.09MPa, and temperature is 85 DEG C；
Step S4, addition nano silica is poured into after mixing carries out ball milling in ball mill, control turning for ball mill
Speed is 2000r/min, and the wear-resisting ink of noctilucence that partial size is 8-13 μm is made.
Comparative example 1
Alkyd resin is not modified by this comparative example compared with Example 1, replaces modified alkyd resin with alkyd resin,
Preparation method is as follows:
Step S1, alkyd resin, polyurethane and half dehydrated alcohol are added in three-necked flask, are heated to 80 DEG C, heat preservation
Nitrogen discharge air is passed through after 1h, control mixing speed is 85r/min, stirs 30min, is warming up to 95 DEG C, keeps the temperature 1h, make A liquid
It is spare；
Step S2, phosphorescent pigment and the other half dehydrated alcohol are added in beaker, 45 DEG C of heating water baths at the uniform velocity stir
Benzoin ethyl ether is added after 15min, is warming up to 75 DEG C, with the revolving speed magnetic agitation 30min of 180r/min, makees B liquid；
Step S3, A liquid is poured into B liquid, at the uniform velocity stirring 5min, dimethicone is added, passes through after ultrasonic disperse 30min
High-speed mixer is stirred, and the revolving speed for controlling blender is 9000r/min, is transferred to drying in vacuum oven after stirring 1h
2h, control vacuum degree are -0.09MPa, and temperature is 85 DEG C；
Step S4, addition nano silica is poured into after mixing carries out ball milling in ball mill, control turning for ball mill
Speed is 2000r/min, and the wear-resisting ink of noctilucence that partial size is 8-13 μm is made.
Comparative example 2
This comparative example compared with Example 1, phosphorescent pigment is not added, and preparation method is as follows:
Step S1, alkyd resin, polyurethane and half dehydrated alcohol are added in three-necked flask, are heated to 80 DEG C, heat preservation
Nitrogen discharge air is passed through after 1h, control mixing speed is 85r/min, stirs 30min, is warming up to 95 DEG C, keeps the temperature 1h, make A liquid
It is spare；
Step S2, the other half dehydrated alcohol is added in beaker, 45 DEG C of heating water baths, peace is added after at the uniform velocity stirring 15min
Fragrant ether is ceased, 75 DEG C is warming up to, with the revolving speed magnetic agitation 30min of 180r/min, makees B liquid；
Step S3, A liquid is poured into B liquid, at the uniform velocity stirring 5min, dimethicone is added, passes through after ultrasonic disperse 30min
High-speed mixer is stirred, and the revolving speed for controlling blender is 9000r/min, is transferred to drying in vacuum oven after stirring 1h
2h, control vacuum degree are -0.09MPa, and temperature is 85 DEG C；
Step S4, addition nano silica is poured into after mixing carries out ball milling in ball mill, control turning for ball mill
Speed is 2000r/min, and the wear-resisting ink of noctilucence that partial size is 8-13 μm is made.
Comparative example 3
This comparative example is a kind of luminous ink in market.
Noctilucence wear-resisting ink sunset glow time prepared by embodiment 1-4 and comparative example 1-3, luminous intensity, wearability and just
Stemness is detected, as a result as shown in table 1 below；
Sunset glow time, luminous intensity: the wear-resisting ink of noctilucence prepared by embodiment 1-4 and comparative example 1-3 is under fluorescent light
After irradiating 5h, sunset glow time, luminous intensity are tested.
Wearability: the embodiment 1-4 and comparative example 1-3 wear-resisting ink samples of noctilucence prepared are cut into 2 × 4cm's respectively
Size is fixed in rubbing table (color of the selected layer of ink to test sample needs more uniform and area to be greater than friction bulk area) and carries out
Friction, observation surface are destroyed situation.
First stemness: referring to GB/T13217.5-2008 " the first stemness method of inspection of liquid ink ", to embodiment 1-4 and comparison
The wear-resisting ink of noctilucence of example 1-3 preparation is detected.
Table 1
It can be seen that the sunset glow time of embodiment 1-4 is between 9.5-12.0h from upper table 1, when the sunset glow of comparative example 1,3
Between between 6.8-9.3h, the 2 sunset glow time of comparative example be 0；The luminous intensity of embodiment 1-4 is in 513-533 (cd/m2) between,
The luminous intensity of comparative example 1,3 is in 455-510 (cd/m2) between, the luminous intensity of comparative example 2 is 0；Embodiment 1,2 and comparison
Example 1 is slight damage in wearability test, and without phenomenon, comparative example 2-3 is then destroyed seriously embodiment 3-4；Embodiment 1-4's is first
Stemness is in 23-31 (μm/30s) range, and the first stemness of comparative example 1-3 is in 15-22 (μm/30s) range.So system of the present invention
The wear-resisting ink of standby noctilucence not only has good noctilucence performance and wear-resisting property, and first stemness is also more excellent.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Above content is only citing made for the present invention and explanation, affiliated those skilled in the art are to being retouched
The specific embodiment stated does various modifications or additions or is substituted in a similar manner, and without departing from invention or surpasses
More range defined in the claims, is within the scope of protection of the invention.
Claims (8)
1. a kind of wear-resisting ink of noctilucence, which is characterized in that be made of following raw material: 35-50 parts of modified alkyd resins,
35-45 parts of phosphorescent pigments, 35-50 parts of polyurethane, 8-15 parts of photoinitiators, 5-12 parts of defoaming agents, 55-70 parts of dehydrated alcohols, 15-
25 parts of nano silicas；
The wear-resisting ink of the noctilucence is made by the following method:
Step S1, modified alkyd resin, polyurethane and half dehydrated alcohol are added in three-necked flask, are heated to 80 DEG C, heat preservation
Nitrogen discharge air is passed through after 1h, control mixing speed is 85r/min, stirs 30min, is warming up to 95 DEG C, keeps the temperature 1h, make A liquid
It is spare；
Step S2, phosphorescent pigment and the other half dehydrated alcohol are added in beaker, 45 DEG C of heating water baths, after at the uniform velocity stirring 15min
Photoinitiator is added, is warming up to 75 DEG C, with the revolving speed magnetic agitation 30min of 180r/min, makees B liquid；
Step S3, A liquid is poured into B liquid, at the uniform velocity stirring 5min, defoaming agent is added, passes through high-speed stirred after ultrasonic disperse 30min
Machine is stirred, and the revolving speed for controlling blender is 9000r/min, is transferred in vacuum oven dry 2h, control after stirring 1h
Vacuum degree is -0.09MPa, and temperature is 85 DEG C；
Step S4, addition nano silica is poured into after mixing carries out ball milling in ball mill, the revolving speed for controlling ball mill is
The wear-resisting ink of noctilucence that partial size is 8-13 μm is made in 2000r/min.
2. the wear-resisting ink of a kind of noctilucence according to claim 1, which is characterized in that the modified alkyd resin by weighing as follows
Amount part raw material is made: 5-8 parts of benzoic acid, 3-5 parts of linoleic acid, 5-10 parts of glutaric anhydrides, 50-75 parts of dimethylbenzene, 10-20 parts of diformazans
Ethylethanolamine, 3-8 parts of sodium peroxydisulfates.
3. the wear-resisting ink of a kind of noctilucence according to claim 1, which is characterized in that the modified alkyd resin is by such as lower section
Method is made:
(1) benzoic acid, linoleic acid, glutaric anhydride and phthalic anhydride are added in the three-necked flask equipped with dimethylbenzene, 50 DEG C
Heating water bath simultaneously at the uniform velocity stirs 20min, and dimethylethanolamine is added, is warming up to 75 DEG C, at the uniform velocity stirring 5min；
(2) it is transferred in the vacuum reaction kettle that vacuum degree is -0.10MPa, is warming up to 150 DEG C and keeps the temperature 2h, observing response kettle goes out
Water is heated up when water yield is stablized with the speed of 5 DEG C/h, until 250 DEG C, it is kept the temperature at this temperature, detects ester
Change degree cools down after being 18mgKOH/g when the acid value of detection, until being down to 30 DEG C, vacuum pumps the dimethylbenzene of reflux, system
Obtain alkyd resin；
(3) alkyd resin is transferred in beaker and is heated to 150 DEG C, addition lauric acid is stirred with the revolving speed magnetic force of 200r/min
30min is mixed, keeps the temperature 45min at this temperature, half sodium peroxydisulfate is added, the other half sodium peroxydisulfate is added after keeping the temperature 1h, is kept the temperature
30min, cooling are added n-butanol up to 60 DEG C, modified alkyd resin are made, and control alkyd resin, lauric acid and n-butanol
Weight ratio is 1: 3: 5.
4. the wear-resisting ink of a kind of noctilucence according to claim 1, which is characterized in that the phosphorescent pigment is by following parts by weight
Raw material is made: 15-28 parts of polyacetylene, 35-45 parts of aniline, 3-8 parts of cadmium yellows, 35-50 parts of glycerine, 3-8 parts of dodecyl sulphates
Sodium, 8-15 parts of ethyl orthosilicates, 3-8 parts of barium sulfate, 5-8 parts of luminescent powders.
5. the wear-resisting ink of a kind of noctilucence according to claim 1, which is characterized in that the phosphorescent pigment is made by the following method
At:
(1) polyacetylene is added in the beaker equipped with half glycerine, is passed through nitrogen to completely cut off air, 60 DEG C of heating water baths
Lauryl sodium sulfate is added in 30min, carries out high speed centrifugation with the revolving speed of 10000r/min after 70 DEG C of heating water bath 5h, will sink
Starch washes of absolute alcohol is clean, is put into 80 DEG C of drying boxes dry 2h, obtains mixture；
(2) ethyl orthosilicate is added in the other half glycerine, 25% ammonium hydroxide is added, triethanolamine is added dropwise after 10min, at the uniform velocity stirs
It mixes until solution is clarified, the weight ratio of control ethyl orthosilicate, 25% ammonium hydroxide and triethanolamine is 5: 0.3: 0.1；
(3) mixture for obtaining step (1) is added in the solution of step (2), after magnetic agitation 1h, is transferred in crucible, according to
Secondary addition aniline, luminescent powder, cadmium yellow and barium sulfate, are warming up to 280 DEG C, heat 5h at this temperature, take out, after standing cooling 1h
Grinding, sieves with 100 mesh sieve, and phosphorescent pigment is made.
6. the wear-resisting ink of a kind of noctilucence according to claim 1, which is characterized in that the photoinitiator is the double first of styrax
One or more of ether, benzoin ethyl ether and benzoin isopropyl ether.
7. the wear-resisting ink of a kind of noctilucence according to claim 1, which is characterized in that the defoaming agent is benzyl carbinol oleic acid
One or more of ester, tributyl phosphate and dimethicone.
8. a kind of preparation method of the wear-resisting ink of noctilucence, which comprises the steps of:
Step S1, modified alkyd resin, polyurethane and half dehydrated alcohol are added in three-necked flask, are heated to 80 DEG C, heat preservation
Nitrogen discharge air is passed through after 1h, control mixing speed is 85r/min, stirs 30min, is warming up to 95 DEG C, keeps the temperature 1h, make A liquid
It is spare；
Step S2, phosphorescent pigment and the other half dehydrated alcohol are added in beaker, 45 DEG C of heating water baths, after at the uniform velocity stirring 15min
Photoinitiator is added, is warming up to 75 DEG C, with the revolving speed magnetic agitation 30min of 180r/min, makees B liquid；
Step S3, A liquid is poured into B liquid, at the uniform velocity stirring 5min, defoaming agent is added, passes through high-speed stirred after ultrasonic disperse 30min
Machine is stirred, and the revolving speed for controlling blender is 9000r/min, is transferred in vacuum oven dry 2h, control after stirring 1h
Vacuum degree is -0.09MPa, and temperature is 85 DEG C；
Step S4, addition nano silica is poured into after mixing carries out ball milling in ball mill, the revolving speed for controlling ball mill is
The wear-resisting ink of noctilucence that partial size is 8-13 μm is made in 2000r/min.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108753031A (en) * | 2017-11-02 | 2018-11-06 | 王小琴 | A kind of ink |
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2019
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108753031A (en) * | 2017-11-02 | 2018-11-06 | 王小琴 | A kind of ink |
Non-Patent Citations (3)
| Title |
|---|
| 何忍事 主编: "《塑胶制品印刷技术》", 31 March 2014, 西安交通大学出版社 * |
| 吴宏富等: "《中国粉体工业通鉴 第三卷（2007版）》", 31 August 2007, 中国建材工业出版社 * |
| 王大全: "《精细化工辞典》", 30 June 1998, 化学工业出版社 * |
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Application publication date: 20190719 |