CN107141888A - A kind of inorganic frit of safety glass ink-jet printing ink and its tempered glass of automobile ink-jet printing ink being formulated - Google Patents
A kind of inorganic frit of safety glass ink-jet printing ink and its tempered glass of automobile ink-jet printing ink being formulated Download PDFInfo
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- CN107141888A CN107141888A CN201710337751.6A CN201710337751A CN107141888A CN 107141888 A CN107141888 A CN 107141888A CN 201710337751 A CN201710337751 A CN 201710337751A CN 107141888 A CN107141888 A CN 107141888A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B27/00—Tempering or quenching glass products
- C03B27/012—Tempering or quenching glass products by heat treatment, e.g. for crystallisation; Heat treatment of glass products before tempering by cooling
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/322—Pigment inks
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/36—Inkjet printing inks based on non-aqueous solvents
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/29—Mixtures
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/119—Deposition methods from solutions or suspensions by printing
Abstract
The invention discloses a kind of inorganic frit of safety glass ink-jet printing ink, the inorganic frit is 100% calculating by its total weight percent, including：25~45% SiO2；15~30% ZnO；10~30% Bi2O3；5~20% B2O3；1~10% K2O；1~10% Na2O；1~10% TiO2；1~10% Li2O；0.1~10%V2O5.The tempered glass of automobile marking ink being formulated using the inorganic frit of the present invention has highly-acidproof and high-sunshade ability, related request of the country to vehicle glass coating acid resistance and sunshade ability can be met, and the fusing point of the inorganic frit can be maintained in 650 ~ 750 DEG C of tempering sintering range, the tempering sintering step in tempered glass of automobile inkjet printing later stage can be enable to be smoothed out.Present invention also offers a kind of tempered glass of automobile ink-jet printing ink being formulated using above-mentioned inorganic frit, it can meet related request of the country to vehicle glass coating acid resistance and sunshade ability.
Description
Technical field
The present invention relates to tempered glass of automobile print field, and in particular to a kind of inorganic frit of glass ink-jet printing ink
And the tempered glass of automobile ink-jet printing ink being formulated using the inorganic frit.
Background technology
The tempered glass of automobile production of current China has formd a huge industry.To reach the mesh kept the sun off
, common processing mode is the dark glass ink of silk-screen printing on tempered glass of automobile.However, the operation of silk-screen printing
It is general complex, it is necessary to which larger human input, the waste material that printing is produced also results in a certain degree of pollution to environment.
In recent years, foreign countries are occurred in that by the way of inkjet printing, and the digital pattern in computer is passed through into shower nozzle noncontact
Formula spray printing glass surface technology.This technology uses special printing device, can print glass marking ink to glass
On the surface of glass, the glass after printing is then sintered into tempering under 650 ~ 750 DEG C of high temperature, ink is merged with glass surface,
It is fixed on the surface of glass.Using this technology, digital pattern can with convenient, fast and accurately print on glass surface,
For a silk-screen printing technique, the artificial operation and material needed for inkjet printing mode are less, and obtained coating quality is high,
Pollution to environment is small.
Existing glass ink-jet printing ink is made up of colorant component, inorganic frit component and organic solvent constituent, colorant
Component and inorganic frit ingredients suspension in organic solvent, constitute suspension.The glass marking ink institute in market is seen at present
The inorganic frit used is classified by its principal component, mainly including SiO2-Bi2O3-B2O3Frit system and SiO2-ZnO-B2O3
Frit system.
Because tempered glass of automobile is throughout the year exposed outside, and it is to block sun in the main function that its surface applies coating
Light, therefore, existing glass ink-jet printing ink are used for there are problems that following both sides during the printing of tempered glass of automobile：
（1）It is unable to reach the highly-acidproof required by tempered glass of automobile：The surface printing of tempered glass of automobile needs to reach state
Highly-acidproof requirement as defined in family standard ASTM C724-91 (2000).The acid resistance of glass ink-jet printing ink is depended primarily on
The acid resistance of inorganic frit.When carrying out acidproof Journal of Sex Research to existing inorganic frit, find to add Ba, Ti class chemical combination in frit
Thing can reach acid proof raising.However, after these compounds are heated, it is found that frit fusing point also can be improved accordingly, causing
Follow-up tempering sintering can not be carried out；
（2）The high hiding rare needed for tempered glass of automobile is not reached：The covering power of coating refers to colored coating to be uniformly coated on
On body surface, the minimum that its background color is no longer presented is set to use cover material amount.For tempered glass of automobile, height is covered as one pleases
Taste high-sunshade ability.The power of glass ink-jet printing ink covering power depends mainly on the following parameter of inorganic frit：
1. refractive index：Coating refractive index is bigger, and covering power is stronger；
2. absorb light ability：The light-absorbing ability of coating is bigger, and covering power is stronger；
3. crystalline substance degree：If can form crystalline form inside inorganic frit, its covering power is stronger；
4. decentralization：The decentralization of suspending components is bigger inside coating, and covering power is stronger.
Glass ink-jet printing ink species at present on the market is seldom, and is to be used to spray multicolour pattern on glass mostly,
It is focus on decoration performances more, such as emphasis be the aesthetic property and durability of color, requirement to the covering power of ink in itself compared with
It is low, it is impossible to reach the requirement needed for tempered glass of automobile.
The content of the invention
The present invention first purpose be to provide a kind of inorganic frit of safety glass ink-jet printing ink, use the nothing
The tempered glass of automobile marking ink that machine frit is formulated has highly-acidproof and high-sunshade ability, can meet country to automobile
The related request of glass coating acid resistance and sunshade ability, and the fusing point of the inorganic frit can be maintained at 650 ~ 750 DEG C of tempering
In sintering range, the tempering sintering step in tempered glass of automobile inkjet printing later stage can be enable to be smoothed out.
Second object of the present invention is to provide a kind of tempered glass of automobile being formulated using above-mentioned inorganic frit
Ink-jet printing ink, it can meet related request of the country to vehicle glass coating acid resistance and sunshade ability.
To reach above-mentioned first purpose, the technical solution adopted by the present invention is as follows：
A kind of inorganic frit of safety glass ink-jet printing ink, described inorganic frit is based on 100% by its total weight percent
Calculate, including：
25~45% SiO2；15~30% ZnO；10~30% Bi2O3；5~20% B2O3;1~10% K2O；1~10% Na2O；1~10%
TiO2；1~10% Li2O；0.1~10%V2O5。
This inorganic frit is to combine existing SiO2-Bi2O3-B2O3Frit system and SiO2-ZnO-B2O3Frit system,
Use SiO simultaneously2、Bi2O3、B2O3With ZnO as principal component, and add K2O、Na2O、TiO2、Li2O and V2O5As being modified to
Point.Inventor has found that the inorganic frit being made of such scheme not only has highly-acidproof through experiment, and its fusing point remains to protect
Hold in 650 ~ 750 DEG C of tempering sintering range, be conducive to the tempering sintering in tempered glass of automobile inkjet printing later stage suitable
Profit is carried out.Wherein, it is in order that obtaining frit has highly-acidproof, but melting temperature can be caused to improve to add titanium oxide；In order to
Overcome this problem, inventor has carried out substantial amounts of experiment and found, is adding a variety of alkalescence such as sodium oxide molybdena, potassium oxide, lithia
After oxide, these oxides have synergy, can make it that the fusing point of inorganic frit is greatly lowered, and the change of frit
Learn stability high.
Simultaneously as the TiO contained in this frit formula2,There is high index of refraction, and V with ZnO2O5It is also that one kind has very
The strong oxide for absorbing light ability, therefore, this frit, which is matched somebody with somebody, can effectively improve the covering power of glass ink-jet printing ink；This
Outside, TiO2Microcrystal can also be formed under certain condition, further improve the glass inkjet printing being made using this glass frit
The covering power of ink.
The present invention can also make following improvement：Described inorganic frit also includes following components：1~10% ZrO2。ZrO2
With high index of refraction, and crystal can be formed.ZrO is further added in this inorganic frit2Afterwards, it can be with original TiO2、ZnO
Etc. collective effect, the covering power of glass ink-jet ink is further improved.
The present invention can also be improved further below：Described inorganic frit also includes following components：0.5~5%
Sb2O3.When carrying out the high-temperature fusion synthesis of glass frit, the air of dissolving is possible to that bubble can be formed inside fused solution, causes
The inorganic frit formed is uneven.The generation of bubble can be reduced by adding antimony oxide, be conducive to being combined to for glass frit.
The present invention can also remake following improvement：Described inorganic frit also includes following components：0.5~10%P2O5。P2O5
Performance and V2O5Performance approach, absorb light ability with strong.P is further added in this inorganic frit2O5Afterwards, its energy
With original V2O5Collective effect, further improves the covering power of glass ink-jet ink.
The inorganic frit of the above-mentioned safety glass ink-jet printing ink of the present invention can be prepared from by following technique：
1. weigh by weight percentage above-mentioned inorganic frit each component and it is well mixed after, 1200 ~
Fused solution is burnt till at 1350 DEG C, and is incubated homogenizing 0.5 ~ 1.5 hour；
2. the fused solution obtained by step 1 is carried out into quenching in 2 ~ 6 DEG C of water, then by the frit obtained after quenching 100 ~
Dried at a temperature of 150 DEG C, obtain inorganic frit.
To reach second above-mentioned purpose, the technical solution adopted by the present invention is as follows：
A kind of tempered glass of automobile ink-jet printing ink being formulated using above-mentioned inorganic frit, it is characterised in that：By gross weight
Percentage is measured to calculate for 100%, including following components in percentage by weight：
The inorganic frit of safety glass ink-jet printing ink described above：20~60%；
Organic solvent：35~65%；
Dispersant：1~15%；
Antistatic additive：0.1~4.5%；
Inorganic pigment component：3.9~35%.
The tempered glass of automobile ink-jet printing ink being formulated using above-mentioned inorganic frit has the advantages that highly-acidproof,
It disclosure satisfy that country is acid proof to tempered glass of automobile coating to require.In addition, as described above, due in inorganic frit formula
It with the addition of the component of high index of refraction, Gao Jingdu and high absorbing ability, the covering power energy of this tempered glass of automobile ink-jet printing ink
It is improved, shaded effects are more preferable.
Specifically, described organic solvent is selected from ethylene glycol, isopropanol, cyclohexanone, butyl acetate, the tert-butyl alcohol, third
Glycol diacetate, dipropylene glycol methyl ether, diethylene glycol monobutyl ether, propylene glycol methyl ether acetate, tripropylene glycol methyl ether, petroleum ether
In one kind or any multiple compounds arbitrary proportion mixing.
Described dispersant can select the wetting dispersing agent and hyper-dispersant suitable for solvent based coating system, and it can increase
The dispersiveness and grain size stability of pigment particles in strong coating, and improve the color acceptance of mill base.For example, can select Germany
Bi Ke chemical companies（BYK-Chemie GmbH）The DISPERBYK-166 of production, DISPERBYK-181, DISPERBYK-163,
BYK-P 104 and Lubrizol Corp. of the U.S.（The Lubrizol Corporation）The Solsperse 8000 that is produced or
The mixing of one kind in Solsperse 20000 or any a variety of arbitrary proportion, more preferably from DISPERBYK-163 or
Solsperse 20000。
Add the dispersant, it is ensured that colored inorganic frit granules is fully dispersed in ink, it is to avoid it is reunited simultaneously
Precipitation, improves the stability of ink, increases the color intensity and covering power of ink.
Described antistatic additive can select ink antistatic additive common on the market, for example, can select and be purchased from Wuxi Ju Wang
JWK-200, JWK-500 of plastifying material Co., Ltd and the CHEMISTAT of SANYO GS chemical conversion industry Co., Ltd. production
One kind in 3500, more preferred with CHEMISTAT 3500.In ink production process, frit is added into dicyandiamide solution simultaneously
It is made after suspension, it is necessary to be ground using sand mill to suspension, the granularity of the solid constituent in suspension is reached one
Fixed standard, it is to avoid block shower nozzle.For a long time（Sometimes need more than 4 hours）Process of lapping in, suspension system is easily produced
Raw electrostatic accumulation.During ink jet print, exist if any electrostatic, easily produce the phenomenon of ink droplet hangover and blocking up for shower nozzle
Plug.Accordingly, it would be desirable to antistatic additive be added, to eliminate the electrostatic gathered in suspension system.
Described inorganic pigment component is one or more coloured metal oxides.
Coloured metal oxide means that the metal oxide of certain color, especially transition are presented at ambient temperature and pressure
The oxide of metal；Its glass colour former well known in the art.During frit is manufactured, by adding appropriate one
Plant or a variety of nonferrous metal oxides, can obtain the frit of different colours.The color of glass ink-jet printing ink generally with it is red,
Based on yellow, primary colors, can also there are black, white either green or other colors as needed.For example, adding oxygen
Changing titanium can make glass frit white, plus nickel oxide can make glass frit in green, and glass frit can be made by adding chrome green
In blueness, glass frit can be made to take on a red color while adding alundum (Al2O3) and chrome green；Addition principal component be titanium dioxide,
The titanium yellow pigment of nickel oxide and antimony oxide can make glass frit be in yellow；By can individually make frit aobvious red, blueness,
Mixing between the metal oxide of yellow, can easily mix the color of other chromas of ink；Added by adjustment
Cobalt oxide and titanium oxide amount, the lightness of ink color can be adjusted.In addition to cited hereinabove, also it can select known
Other metal oxides with glass hair color effect, such as iron oxide, cuprous oxide, manganese oxide.
It is highly preferred that described inorganic pigment component is copper-chrome black（Cr2CuO4）.
Black is presented in copper-chrome black, with the effect of blocking to sunlight, it is adaptable to tempered glass of automobile.
Specifically, the maximum particle diameter of the inorganic frit in described glass ink-jet printing ink is<1.3um, average grain
Footpath is 300 ~ 700nm.
Specifically, viscosity of the described tempered glass of automobile ink-jet printing ink under injection temperation is 9 ~ 18 lis of handkerchiefs.
The above-mentioned tempered glass of automobile ink-jet printing ink of the present invention can be prepared from by following technique：
1. method as described above, prepares the inorganic frit of safety glass ink-jet printing ink；
2. using ball mill, inorganic frit and the inorganic pigment component that percentage by weight is identified above are subjected to ball milling together, made
The average grain diameter for obtaining the inorganic frit mixed powder obtained after ball milling is 30 ~ 40um；
3. fixed percentage by weight weighs and prepares organic solvent, dispersant and antistatic additive respectively as addressed above, mixed
Close liquid；
4. the inorganic frit mixed powder obtained by step 2 is added in the mixed liquor obtained by step 3, in dispersion machine with 1500 ~
2500rpm is stirred at least 20 minutes, obtains suspension；
It is ground 5. the suspension obtained by step 4 is poured into sand mill, makes the average grain diameter of the solid constituent in suspension
≤ 0.45um, d90≤1.25um；D herein90Mean that the cumulative particle sizes percentile of glass ink-jet print water sample reaches
Particle diameter is less than d in corresponding particle diameter, i.e. sample during to 90%90Particle account for 90%.
6. the suspension after this is ground is filtered by filter, glass ink-jet printing ink is obtained.
The invention has the advantages that：
（1）The inorganic frit of the present invention not only has highly-acidproof, and its fusing point remains to be maintained at 650 ~ 750 DEG C of tempering sintering
In temperature range, glass ink-jet printing ink is set to be smoothed out tempering sintering after inkjet printing；
（2）The glass ink-jet printing ink being made using the inorganic frit of the present invention has highly-acidproof, disclosure satisfy that country is right
The acid proof related request of vehicle glass coating；
（3）By the component of addition high index of refraction, Gao Jingdu and high absorbing ability in inorganic frit formula, the ink-jet of this glass is beaten
The covering power of printing ink can effectively improve, and shaded effects of the tempered glass of automobile after inkjet printing are good；
（4）The proportion of the inorganic frit of the present invention is lighter, is only about 3g/ML, is being ground to average grain diameter≤0.45um, d90≤
There is good suspension in organic solvent after 1.25um；
（5）Compared with existing inorganic frit, the inorganic frit of the invention Bi higher due to reducing cost2O3Content,
Therefore the preparation cost of frit is significantly reduced.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described.
In following embodiments, used Bi2O3The bismuth oxide that preferably Guangzhou Chemical Reagent Factory is produced；Used
SiO2The silica that preferably Guangzhou Chemical Reagent Factory is produced（Heavy）；Used B2O3Preferably Chengdu bass spy examination
The boron oxide of agent Co., Ltd production（B000554）；Used ZrO2The preferably special reagent Co., Ltd production of Chengdu bass
Zirconium dioxide（B007669）；Used citric acid is preferably the citric acid of Guangzhou Chemical Reagent Factory production；It is used
K2O is prepared from by heat resolve potassium nitrate, and used potassium nitrate is preferably the potassium nitrate of Guangzhou Chemical Reagent Factory production；
Used concentrated hydrochloric acid solution is preferably the 37wt% hydrochloric acid solutions of lark prestige Science and Technology Ltd. production；Used TiO2It is excellent
Elect 99.8% titanium oxide of lark prestige Science and Technology Ltd. production as；Used Na2O is preferably lark prestige Science and Technology Ltd.
The sodium oxide molybdena of production；Used Li2O is preferably 98.5% lithia of lark prestige Science and Technology Ltd. production；It is used
ZnO is preferably the zinc oxide of Guangzhou Chemical Reagent Factory production；Used barium monoxide is preferably the life of lark prestige Science and Technology Ltd.
The BaO of production（≥99%）；Used V2O5The vanadic anhydride that preferably Guangzhou Chemical Reagent Factory is produced；Used P2O5It is excellent
Elect the P of lark prestige Science and Technology Ltd. production as2O5（98%）；Used copper-chrome black is produced by Xue Te pigment company of the U.S.；Institute
DISPERBYK-166, DISPERBYK-181, DISPERBYK-163 and the BYK-P 104 used is Bi Ke chemistry（Tongling）
The dispersant that Co., Ltd is produced；Used Solsperse 8000 and Solsperse 20000 are Lubrizol Corp.
The pigment dispersing agent of the Solsperse series produced；Used JWK-200 and JWK-500 are purchased from Wuxi Ju Wang
The antistatic additive of plastifying material Co., Ltd；Used CHEMISTAT 3500 is institute of SANYO GS chemical conversion industry Co., Ltd.
The antistatic additive of production；Used ethylene glycol is preferably 99.5% ethylene glycol of lark prestige Science and Technology Ltd. production；Used
Isopropanol be preferably lark prestige Science and Technology Ltd. production 99.7% isopropanol；Used cyclohexanone is preferably lark prestige
99.5% cyclohexanone of Science and Technology Ltd.'s production；Used butyl acetate is preferably that lark prestige Science and Technology Ltd. produces
99% n-butyl acetate；The used tert-butyl alcohol is preferably the tert-butyl alcohol of lark prestige Science and Technology Ltd. production（>99%）；Used
Propylene-glycol diacetate be preferably lark prestige Science and Technology Ltd. production 98% propylene-glycol diacetate；Used dipropyl
Glycol methyl ether is preferably 99.5% dipropylene glycol monomethyl ether of lark prestige Science and Technology Ltd. production（Isomer mixture）；Made
Diethylene glycol monobutyl ether is preferably the uncommon love of ladder（Shanghai）The diethylene glycol monobutyl ether of chemical conversion industry Development Co., Ltd production
（>98.0%）；Used propylene glycol methyl ether acetate is preferably 99% propane diols list first of lark prestige Science and Technology Ltd. production
Ether acetic acid ester；Used tripropylene glycol methyl ether is preferably 98% 1- [2- (the 2- methoxies of lark prestige Science and Technology Ltd. production
Base -1- methyl ethoxies) -1- methyl ethoxies] -2- propyl alcohol（Isomer mixture）；Used petroleum ether is preferably lark
The petroleum ether of prestige Science and Technology Ltd. production（extra pure, boiling range 40-60℃）；Used drying oven
The box coloring drying oven that preferably Shijiazhuang Wu Feng thermal technologies Machinery Co., Ltd. produces；Used ball mill is preferably Nanjing
The QM-KD low temperature-controlled planetary ball mills of Nan great Instrument Ltd. production, mill pearl selects 10 millimeters of high aluminium ball；Used
Disk high speed dispersor be preferably Sichuan Chang Xinyuan plant equipment Co., Ltd production high speed dispersor CGF-11；Used
Sand mill be preferably resistance to speed（Shanghai）The vertical sand mill KE of mechanical device Co., Ltd production；Used filter is excellent
Elect the H-CCF single technical grade liquid filters of Hangzhou Cobetter Filtration Equipment Co., Ltd.'s production as, filter core is 5 microns；Remove
It is above-mentioned enumerate outside, those skilled in the art according to conventional selection, can also select it is other have with the present invention enumerate it is upper
Stating product has the product of similar performance, can realize the purpose of the present invention.
Unless otherwise noted, the percentage in context is percetage by weight.
In examples below, prepared glass ink-jet printing ink is tested by following experiment：
The acid resistance test carried out according to national standard ASTM C724-91 (2000)
（1）By prepared glass ink-jet printing ink through on inkjet printing to the thick tempered glass of automobile of 5mm after cleaned, warp
680 DEG C it is High temperature tempered processing 3.5 minutes；
（2）Prepare 10wt% citric acid solution：In the distilled water that the citric acid of 10 parts by weight is dissolved in 90 parts by weight；
（3）Prepare 3.7wt% hydrochloric acid solution：By the concentrated hydrochloric acid solution of 10 parts by weight（37wt%）It is dissolved in the distillation of 90 parts by weight
Water；
（4）Difference is chosen on tested tempered glass of automobile two kinds of above-mentioned acid solutions, every kind of acid solution are added dropwise respectively
Respectively plus four to drip, often drop chooses different points, every cap upper surface ware prevents solution from evaporating, 20 ± 2 DEG C of holding 15min；
（5）After 15min, acid solution is washed down with running water, tested tempered glass of automobile is dried naturally, and in magnifying glass
Under it is observed.
Embodiment 1
A kind of inorganic frit of safety glass ink-jet printing ink, is 100% calculating by its total weight percent, including with the following group
Point：
25% SiO2、15% ZnO、10% Bi2O3、20% B2O3、10% K2O、10% Na2O、5% ZrO2、1% Li2O、1%TiO2、
3%V2O5。
A kind of glass ink-jet printing ink being formulated using above-mentioned inorganic frit, is 100% by its total weight percent
Calculate, including following components：
Inorganic frit：20%th, organic solvent：65%th, dispersant：1%th, antistatic additive：0.1%th, copper-chrome black：13.9%.
Described dispersant selects Solsperse 20000, and described antistatic additive selects CHEMSTAT3500.
Counted using the total weight percent of organic solvent as 100%, it includes following component calculated in weight percent：It is different
Propyl alcohol：48.6%th, butyl acetate：11%th, cyclohexanone：24%th, diethylene glycol monobutyl ether：11.4%th, petroleum ether 5%.
Prepare the step of above-mentioned inorganic frit formula prepares glass/ceramic ink-jet printing ink as follows：
1. after weighing each component of above-mentioned inorganic frit by weight percentage and being well mixed, it is positioned over smelting furnace fused alumina zirconia
In in the tank furnace built by laying bricks or stones, fused solution is burnt till at 1280 DEG C, and be incubated homogenizing one hour；
2. the fused solution obtained by step 1 is carried out into quenching in 4 DEG C of water, the frit obtained after quenching is then delivered to 100 DEG C
Drying oven in be dried.Using ball mill, ball milling is carried out to inorganic frit and copper-chrome black so that what is obtained after ball milling is inorganic
The average grain diameter of frit mixed powder is 35 μm；
3. the percentage by weight as specified by the present embodiment weighs and configures organic solvent, dispersant and antistatic additive, mixed
Close liquid；
4. the inorganic frit mixed powder and colorant component obtained by step 2 are added in the mixed liquor obtained by step 3, it is high in disk
Stirred 20 minutes with 2000rpm in fast dispersion machine, obtain suspension；
It is ground 5. the suspension obtained by step 4 is poured into sand mill, makes the average grain diameter of the solid constituent in suspension
For 0.45um, d90For 1.25um；
6. the suspension after this is ground is filtered by filter, glass ink-jet printing ink is obtained.
Using method as discussed above, the acid resistance to resulting ink is tested.After a test, it was observed that
There is not obvious corrosion phenomenon in sample, and be up to state standards acid resistances of the ASTM C724-91 (2000) to tempered glass of automobile
It is required that.
Embodiment 2
A kind of inorganic frit of safety glass ink-jet printing ink, is 100% calculating by its total weight percent, including with the following group
Point：
45% SiO2、30% ZnO、15% Bi2O3、5% B2O3、1% K2O、1% Na2O、1% Li2O。0.1%V2O5；1.9%TiO2。
A kind of glass ink-jet printing ink being formulated using above-mentioned inorganic frit, is 100% by its total weight percent
Calculate, including following components：
Inorganic frit：60%；Organic solvent：35%；Dispersant：1%；Antistatic additive：0.1%th, copper-chrome black：3.9%.
Described dispersant selects Solsperse 20000, and described antistatic additive selects CHEMSTAT3500.
Counted using the total weight percent of organic solvent as 100%, it includes following component calculated in weight percent：Ring
Hexanone：24%；Dipropylene glycol methyl ether：48.6%；Propylene-glycol diacetate：12%；Diethylene glycol monobutyl ether：10.4%；Petroleum ether：
5%。
The glass ink-jet printing ink for manufacturing the present embodiment is comprised the following steps that：
1. after weighing each component of above-mentioned inorganic coloured frit by weight percentage and being well mixed, it is positioned over smelting furnace zirconium
In in the tank furnace that corundum is built by laying bricks or stones, fused solution is burnt till at 1200 DEG C, and be incubated homogenizing 1.5 hours；
2. the fused solution obtained by step 1 is carried out into quenching in 2 DEG C of water, the frit obtained after quenching is then delivered to 150 DEG C
Drying oven in be dried.Using ball mill, ball milling is carried out to inorganic frit and copper-chrome black so that what is obtained after ball milling is inorganic
The average grain diameter of frit mixed powder is 30 μm；
3. fixed percentage by weight weighs and organic solvent, dispersant and antistatic additive is respectively configured as addressed above, mixed
Close liquid；
4. the inorganic coloured frit powder obtained by step 2 is added in the mixed liquor obtained by step 3, in disk high speed dispersor
Stirred 30 minutes with 1500rpm, obtain suspension；
It is ground 5. the suspension obtained by step 4 is poured into sand mill, makes the average grain diameter of the solid constituent in suspension
For 0.35 μm, d90For 1.15 μm；
6. the suspension after this is ground is filtered by filter, glass ink-jet printing ink is obtained.
Using method as discussed above, the acid resistance to resulting ink is tested.After a test, it was observed that
There is not obvious corrosion phenomenon in sample, and be up to state standards acid resistances of the ASTM C724-91 (2000) to tempered glass of automobile
It is required that.
Embodiment 3
A kind of inorganic frit of safety glass ink-jet printing ink, is 100% calculating by its total weight percent, including with the following group
Point：
30% SiO2、20% ZnO、30% Bi2O3、10% B2O3、1.5% K2O、2% Na2O、2%TiO2、2%Li2O、2.5%V2O5.
A kind of glass ink-jet printing ink being formulated using above-mentioned inorganic frit, is based on 100% by its total weight percent
Calculate, including following components：
Inorganic coloured frit：25%；Organic solvent：45%；Dispersant：15%；Antistatic additive：4.5%；Copper-chrome black：10.5%.
DISPERBYK-163 of the described dispersant from 0.7% Solsperse 8000 and 0.3%；Described is anti-quiet
JWK-200 is selected in electric agent, and described organic solvent is ethylene glycol.
The glass ink-jet printing ink for manufacturing the present embodiment is comprised the following steps that：
1. after weighing each component of above-mentioned inorganic frit by weight percentage and being well mixed, it is positioned over smelting furnace fused alumina zirconia
In in the tank furnace built by laying bricks or stones, fused solution is burnt till at 1300 DEG C, and be incubated homogenizing 0.5 hour；
2. the fused solution obtained by step 1 is carried out into quenching in 6 DEG C of water, the frit obtained after quenching is then delivered to 100 DEG C
Drying oven in be dried.Using ball mill, ball milling is carried out to inorganic frit and copper-chrome black so that what is obtained after ball milling is inorganic
The average grain diameter of coloured frit powder is 40 μm；
3. fixed percentage by weight weighs and organic solvent, dispersant and antistatic additive is respectively configured as addressed above, mixed
Close liquid；
4. the inorganic coloured frit powder obtained by step 2 is added in the mixed liquor obtained by step 3, in disk high speed dispersor
Stirred 30 minutes with 2500rpm, obtain suspension；
It is ground 5. the suspension obtained by step 4 is poured into sand mill, makes the average grain diameter of the solid constituent in suspension
For 0.25 μm, d90For 1.00 μm；
6. the suspension after this is ground is filtered by filter, glass ink-jet printing ink is obtained.
Using method as discussed above, the acid resistance to resulting ink is tested.After a test, it was observed that
There is not obvious corrosion phenomenon in sample, and be up to state standards acid resistances of the ASTM C724-91 (2000) to tempered glass of automobile
It is required that.
Embodiment 4
A kind of inorganic frit of safety glass ink-jet printing ink, is 100% calculating by its total weight percent, including with the following group
Point：
26% SiO2、16% ZnO、21%Bi2O3、6%B2O3、4%K2O、5%Na2O、10%TiO2、10%Li2O、2%V2O5。
A kind of glass ink-jet printing ink being formulated using above-mentioned inorganic frit, is 100% by its total weight percent
Calculate, including following components：
Inorganic coloured frit：20%；Organic solvent：40%；Dispersant：3%；Antistatic additive：2%；Copper-chrome black：35%.
Described dispersant selects 0.9%DISPERBYK-166,1.2%DISPERBYK-181 and 0.9%BYK-P 104, institute
The antistatic additive stated selects JWK-500, and described organic solvent is propylene glycol methyl ether acetate.
The glass ink-jet printing ink for manufacturing the present embodiment is comprised the following steps that：
1. after weighing each component of above-mentioned inorganic coloured frit by weight percentage and being well mixed, it is positioned over smelting furnace zirconium
In in the tank furnace that corundum is built by laying bricks or stones, fused solution is burnt till at 1250 DEG C, and be incubated homogenizing one hour；
2. the fused solution obtained by step 1 is carried out into quenching in 4 DEG C of water, the frit obtained after quenching is then delivered to 140 DEG C
Drying oven in be dried.Using ball mill, ball milling is carried out to inorganic frit and copper-chrome black so that what is obtained after ball milling is inorganic
The average grain diameter of coloured frit powder is 33 μm；
3. fixed percentage by weight weighs and organic solvent, dispersant and antistatic additive is respectively configured as addressed above, mixed
Close liquid；
4. the inorganic coloured frit powder obtained by step 2 is added in the mixed liquor obtained by step 3, in disk high speed dispersor
Stirred 25 minutes with 2200rpm, obtain suspension；
It is ground 5. the suspension obtained by step 4 is poured into sand mill, makes the average grain diameter of the solid constituent in suspension
For 0.45 μm, d90For 1.25 μm；
6. the suspension after this is ground is filtered by filter, glass ink-jet printing ink is obtained.
Using method as discussed above, the acid resistance to resulting ink is tested.After a test, it was observed that
There is not obvious corrosion phenomenon in sample, and be up to state standards acid resistances of the ASTM C724-91 (2000) to tempered glass of automobile
It is required that.
Embodiment 5
A kind of inorganic frit of safety glass ink-jet printing ink, is 100% calculating by its total weight percent, including with the following group
Point：
33% SiO2、16% ZnO、11% Bi2O3、8% B2O3、2% K2O、6% Na2O、10% V2O5、4% Li2O、10% TiO2。
A kind of glass ink-jet printing ink being formulated using above-mentioned inorganic frit, is 100% by its total weight percent
Calculate, including following components：
Inorganic frit：49%；Organic solvent：35%；Dispersant：10%；Antistatic additive：0.1%；Siderochrome is black：5.9%.
Described dispersant selects DISPERBYK-166；Described antistatic additive selects JWK-200.
Counted using the total weight percent of organic solvent as 100%, it includes following component calculated in weight percent：30%
Propylene glycol methyl ether acetate, 70% tripropylene glycol methyl ether.
Method according to embodiment 1 prepares the glass ink-jet printing ink of the present embodiment.
Using method as discussed above, the acid resistance to resulting ink is tested.After a test, it was observed that
There is not obvious corrosion phenomenon in sample, and be up to state standards acid resistances of the ASTM C724-91 (2000) to tempered glass of automobile
It is required that.
Embodiment 6
A kind of inorganic frit of safety glass ink-jet printing ink, is 100% calculating by its total weight percent, including with the following group
Point：
25%SiO2、15% ZnO、10% Bi2O3、5% B2O3、1% K2O、1% Na2O、6% TiO2、1% Li2O、1% V2O5、10%
BaO、10%ZrO2、10%P2O5、5%Sb2O3。
A kind of glass ink-jet printing ink being formulated using above-mentioned inorganic frit, is 100% by its total weight percent
Calculate, including following components：
Inorganic frit：27%；Organic solvent：36%；Dispersant：10%；Antistatic additive：4%；Copper-chrome black：23%.
Described dispersant selects the and of 0.2%DISPERBYK-181,0.6%DISPERBYK-163,1.0%BYK-P 104
0.2%Solsperse 20000；Described antistatic additive selects CHEMISTAT 3500.
Counted using the total weight percent of organic solvent as 100%, it includes following component calculated in weight percent：23%
Butyl acetate, 42% tert-butyl alcohol and 35% dipropylene glycol methyl ether.
Method according to embodiment 1 prepares the glass ink-jet printing ink of the present embodiment.
Using method as discussed above, the acid resistance to resulting ink is tested.After a test, it was observed that
There is not obvious corrosion phenomenon in sample, and be up to state standards acid resistances of the ASTM C724-91 (2000) to tempered glass of automobile
It is required that.
Embodiment 7
A kind of inorganic frit of safety glass ink-jet printing ink, is 100% calculating by its total weight percent, including with the following group
Point：
40% SiO2、15% ZnO、10% Bi2O3、5% B2O3、5% K2O、5% Na2O、1% ZrO2、10% Li2O、7% TiO2、
0.5% Sb2O3、1% V2O5、0.5% P2O5。
A kind of glass ink-jet printing ink being formulated using above-mentioned inorganic frit, is 100% by its total weight percent
Calculate, including following components：
Inorganic frit：46%；Organic solvent：35%；Dispersant：10%；Antistatic additive：3%；Copper-chrome black：6%.
Described dispersant selects 3%BYK-P 104 and 7%Solsperse 8000；Described antistatic additive selects JWK-
500。
Counted using the total weight percent of organic solvent as 100%, it includes following component calculated in weight percent：10%
Ethylene glycol, 15% isopropanol, 21% tert-butyl alcohol, 35% diethylene glycol monobutyl ether, 13% tripropylene glycol methyl ether and 6% petroleum ether.
Method according to embodiment 1 prepares the glass ink-jet printing ink of the present embodiment.
Using method as discussed above, the acid resistance to resulting ink is tested.After a test, it was observed that
There is not obvious corrosion phenomenon in sample, and be up to state standards acid resistances of the ASTM C724-91 (2000) to tempered glass of automobile
It is required that.
Embodiment 8
A kind of inorganic frit of safety glass ink-jet printing ink, is 100% calculating by its total weight percent, including with the following group
Point：
30%SiO2、20%ZnO、20%Bi2O3、10%B2O3、8%K2O、4%Na2O、4%TiO2、2%Li2O、1%V2O5、1%BaO。
A kind of glass ink-jet printing ink being formulated using above-mentioned inorganic frit, is 100% by its total weight percent
Calculate, including following components：
Inorganic frit：46%；Organic solvent：35%；Dispersant：10%；Antistatic additive：3%；Copper-chrome black：6%.
Described dispersant selects 3%BYK-P 104 and 7%Solsperse 8000；Described antistatic additive selects JWK-
500。
Counted using the total weight percent of organic solvent as 100%, it includes following component calculated in weight percent：10%
Ethylene glycol, 15% isopropanol, 21% tert-butyl alcohol, 35% diethylene glycol monobutyl ether, 13% tripropylene glycol methyl ether and 6% petroleum ether.
Method according to embodiment 1 prepares the glass ink-jet printing ink of the present embodiment.
Using method as discussed above, the acid resistance to resulting ink is tested.After a test, it was observed that
There is not obvious corrosion phenomenon in sample, and be up to state standards acid resistances of the ASTM C724-91 (2000) to tempered glass of automobile
It is required that.
Claims (10)
1. a kind of inorganic frit of safety glass ink-jet printing ink, it is characterised in that：Described inorganic frit presses its gross weight
Percentage is 100% calculating, including：25~45% SiO2；15~30% ZnO；10~30% Bi2O3；5~20% B2O3；1~10% K2O；
1~10% Na2O；1~10% TiO2；1~10% Li2O；0.1~10%V2O5。
2. the inorganic frit of safety glass ink-jet printing ink according to claim 1, it is characterised in that：Described is inorganic
Frit also includes 1 ~ 10% ZrO2。
3. the inorganic frit of safety glass ink-jet printing ink according to claim 1, it is characterised in that：Described is inorganic
Frit also includes 0.5 ~ 5% Sb2O3。
4. the inorganic frit of safety glass ink-jet printing ink according to claim 1, it is characterised in that：Described is inorganic
Frit also includes 0.5 ~ 10%P2O5。
5. one kind is matched somebody with somebody using the inorganic frit of the safety glass ink-jet printing ink according to any one in claim 1 ~ 4
The tempered glass of automobile ink-jet printing ink of system, it is characterised in that：By total weight percent be 100% calculate, it include with
The component of lower percentage by weight：The inorganic frit of described safety glass ink-jet printing ink：20~60%；Organic solvent：35~
65%；Dispersant：1~15%；Antistatic additive：0.1~4.5%；Inorganic pigment component：3.9~35%.
6. the vapour that the inorganic frit according to claim 5 using described safety glass ink-jet printing ink is formulated
Car safety glass ink-jet printing ink, it is characterised in that：Described organic solvent is selected from ethylene glycol, isopropanol, cyclohexanone, vinegar
Acid butyl ester, the tert-butyl alcohol, propylene-glycol diacetate, dipropylene glycol methyl ether, diethylene glycol monobutyl ether, propylene glycol methyl ether acetate, three
The mixing of the arbitrary proportion of one kind or any multiple compounds in propylene glycol monomethyl ether, petroleum ether；Described dispersant is market
The upper common wetting dispersing agent and hyper-dispersant suitable for solvent based coating system；Described antistatic additive is that ink is quiet with resisting
Electric agent.
7. the vapour that the inorganic frit according to claim 5 using described safety glass ink-jet printing ink is formulated
Car safety glass ink-jet printing ink, it is characterised in that：Described inorganic pigment component is one or more coloured metal oxygens
Compound.
8. the vapour that the inorganic frit according to claim 7 using described safety glass ink-jet printing ink is formulated
Car safety glass ink-jet printing ink, it is characterised in that：Described inorganic pigment component is copper-chrome black.
9. the vapour that the inorganic frit according to claim 5 using described safety glass ink-jet printing ink is formulated
Car safety glass ink-jet printing ink, it is characterised in that：The maximum of the inorganic frit of described safety glass ink-jet printing ink
Particle diameter is<1.3um, average grain diameter is 300 ~ 700nm.
What 10. the inorganic frit according to claim 5 using described safety glass ink-jet printing ink was formulated
Tempered glass of automobile ink-jet printing ink, it is characterised in that：Its viscosity under injection temperation is 9 ~ 18 lis of handkerchiefs.
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Effective date of registration: 20190325 Address after: 315506 East Side of No.7 Workshop in Binhai New Area, Fenghua Economic Development Zone, Ningbo City, Zhejiang Province Patentee after: Ningbo Meike Digital Intelligent Technology Co., Ltd. Address before: 510530 No. 11 B9-416 Kaiyuan Avenue, Guangzhou Economic and Technological Development Zone, Guangzhou, Guangdong Province Patentee before: Guangzhou City Chemical Material Technology Co Ltd |