CN106752376A - A kind of oiliness ceramics ooze colored color development ink toner and its preparation and usage - Google Patents
A kind of oiliness ceramics ooze colored color development ink toner and its preparation and usage Download PDFInfo
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- CN106752376A CN106752376A CN201611243299.9A CN201611243299A CN106752376A CN 106752376 A CN106752376 A CN 106752376A CN 201611243299 A CN201611243299 A CN 201611243299A CN 106752376 A CN106752376 A CN 106752376A
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- color development
- oiliness
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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
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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
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Ink Jet Recording Methods And Recording Media Thereof (AREA)
Abstract
The invention belongs to figure punch Material Field, and in particular to a kind of oiliness ceramics ooze colored color development ink toner and its preparation and usage.The toner is made up of the organic solvent of the hyperchromic metallic compounds of 50~95wt% and 50~5wt%, and the hyperchromic metallic compound is at least one in the organic compound of antimony, titanium, zirconium, zinc and tin；The organic solvent is at least one in acids solvent, varsol and esters solvent.The toner and color development ink are pressed 4~50:After 100 mass ratio is well mixed at room temperature, it is printed upon by digital ink-jet in ceramic body or glaze paint by gained filtrate after less than 5 μm of filter opening filtering, by high temperature, 650~1250 DEG C are burnt till 4~1 hours, color development ink stabilization is manifested various patterns, can also increase color development vividness.
Description
Technical field
The invention belongs to figure punch Material Field, and in particular to a kind of oiliness ceramics ooze colored color development ink toner and its
Prepare and usage.
Background technology
The high speed development of digital technology greatly improves the quality of printing technique and promotes the use of.Ceramic digital ink-jet printing
Technology is a kind of ceramic surface decoration technique, by Computer Design can convenient and swift automatic printing into various patterns so that pottery
Tile product pattern more horn of plenty, true to nature, personalized and rich unlimited creativity.
It is a kind of low viscosity osmosis type ink that colored color development ink is oozed in ceramic digital ink-jet printing, and colour former is mainly molten by energy
The organic metal of chromium, manganese, iron, cobalt, nickel, copper, osmium, iridium, platinum, ruthenium, rhodium, palladium, gold, silver and lanthanide rare metal in organic solvent
Salt is constituted.Color development ink has the ability of diffusion after printing of inkjet printer in Ceramic Tiles frit surface, by high temperature
Burn till, colour former is converted at high temperature can be presented the metal oxide of color, form the pre-designed pattern of computer.But,
In high temperature sintering process, color development metallic compound can occur a series of chemical reaction, typically result in metal oxide color development not
Stabilization is even unable to color development.For this problem, China applies for a patent CN201510429407.0, and (a kind of ink-jet is oozed colored Ceramic Tiles and is increased
Toner and application method) superfine silicon dioxide as Ceramic glaze powder additive is described as toner, but resistance to height
Mixed interface between the other colour former of pelletized silica and molecular level of temperature is very it will be evident that have impact on hair to a certain degree
The uniformity of color.The other toner of colored color development ink oil-soluble molecular level is oozed in oiliness ceramics on directly addition, not
Document report.
The content of the invention
Primary and foremost purpose of the invention is to provide a kind of digital ink-jet printing pottery that can directly add in oiliness color development ink
Porcelain oozes colored color development ink toner (i.e. oiliness ceramics ooze colored color development ink toner).
The preparation method of colored color development ink toner is oozed another object of the present invention is to provide above-mentioned oiliness ceramics.
Another object of the present invention is to provide the application method that above-mentioned oiliness ceramics ooze colored color development ink toner.
The purpose of the present invention is achieved through the following technical solutions：
A kind of oiliness ceramics ooze colored color development ink toner, the toner by the hyperchromic metallic compounds of 50~95wt% and
50~5wt% organic solvent composition, the hyperchromic metallic compound for antimony, titanium, zirconium, zinc and tin organic compound in extremely
Few one kind, the organic solvent is at least one in acids solvent, varsol and esters solvent.
Preferably, the hyperchromic metallic compound is the oxygen/sulphur ligand complex of antimony, the carboxylic acid alkoxide compound of titanium
((RO)mM(OOC-R’)n, m, n are the integer more than or equal to 1 in formula, and R is ethyl, propyl group, isopropyl or butyl, and R ' is C7
~C9Alkyl), the ethylhexanoate salt of zirconium, the ethylhexanoate salt of zinc, neodecanoate, in the ethylhexanoate salt and dibutyl tin laurate of tin
At least one；
It is furthermore preferred that described oxygen/sulphur part is containing aerobic or element sulphur ligand compound, including isooctyl acid, Malaysia
Sour mono-n-butylester, Malaysia monooctyl acid monooctyl ester, the different monooctyl ester of succinic acid list, the different monooctyl ester of adipic acid list, the different monooctyl ester of decanedioic acid list, O-phthalic
Monooctyl acid monooctyl ester or isooctyl thioglycolate.
Preferably, described organic solvent is isooctyl acid, neodecanoic acid, C7~C20Liquid long chain alkane, tricaprylate, the new last of the ten Heavenly stems
At least one in acid esters, long alkyl chain methacrylates and acrylate long-chain ester.
Above-mentioned oiliness ceramics ooze the preparation method of colored color development ink toner, comprise the following steps：By hyperchromic metal compound
Thing is well mixed with organic solvent at room temperature, that is, obtain the liquid digital ink-jet printing oiliness ceramics that pH value is 4~7 and ooze Hua Mo
Water toner (i.e. oiliness ceramics ooze colored color development ink toner).
Room temperature of the present invention is 15~35 DEG C.
Above-mentioned oiliness ceramics ooze the application method of colored color development ink toner, comprise the following steps：
(1) oiliness ceramics are oozed into colored color development ink toner with oiliness color development ink by 4~50:100 quality compares room temperature
It is lower well mixed, to be filtered by less than 5 μm of filter openings, gained filtrate is printed upon ceramic body or base substrate glaze surface through digital ink-jet
On；
(2) high temperature for being dried with 650~1250 DEG C by infiltration again burns till 1~4 hour, color development ink stabilization is manifested each
Bright-coloured pattern is planted, bright-coloured pattern is showed after cooling.
It is that the hyperchromic metallic compound of molecular state is molten that oiliness ceramics prepared by the present invention ooze colored color development ink toner
Solution dispersion is in organic solvent, compatible very well with oil type color development ink, miscible with molecule rank each other.Printed by digital ink-jet
After ceramic body or base substrate glaze surface, by permeating drying, hyperchromic metallic compound and color development metallic compound still keep
Well mixed state, then the metal oxide of the uniform hydridization of atom and molecule is formed by high temperature sintering, the pattern of stabilization is presented, and
There is significant hyperchromic effect to color development metal oxide.
Compared with prior art, the present invention has following prominent distinguishing feature and advantage：
(1) oiliness ceramics of the present invention ooze colored color development ink toner and are easily well mixed with color development ink；
(2) to ooze the easy inkjet printing of ink after colored color development ink toner mixes with color development ink equal for oiliness ceramics of the present invention
Even, permeability is consistent, and high temperature burns till color development stable and uniform, and dramatically increases the vividness that color development ink is in pattern.
Brief description of the drawings
Fig. 1 is the EDS elementary analysis figures of three (isooctyl thioglycolate) antimony.
Fig. 2 is the infrared spectrogram of three (isooctyl thioglycolate) antimony.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited
In this.Methods described is conventional method unless otherwise instructed, and the raw material unless otherwise instructed can be from open commercial sources
And obtain.
Embodiment 1：The preparation of oiliness antimony system color development ink toner raw material
The preparation of (1) three (isooctyl thioglycolate) antimony：61.30g (0.3mol) TGA is added in round-bottomed flask
Different monooctyl ester, 13.25g (0.045mol) antimony oxides and 45g water, magnetic agitation, 80 DEG C of back flow reaction 2h, by dividing after cooling
Liquid funnel point liquid, removes upper strata aqueous phase；Lower floor's organic phase is distilled by circulating water type vacuum pump pressure, and removing is remained in oil phase
Water, obtain oiliness antimony system color development ink toner raw material ----three (isooctyl thioglycolate) antimony YSb1, it is standby.Then test
Its elementary analysis and infrared spectrum, respectively obtain Fig. 1 and Fig. 2.
Fig. 1 is the EDS elementary analysis figures of three (isooctyl thioglycolate) antimony, according to EDS elementary analyses, target product three
The content of antimony is 19.11wt% in (isooctyl thioglycolate) antimony.
Fig. 2 is the infrared spectrogram of three (isooctyl thioglycolate) antimony.2950cm-1, 2930cm-1, 2860cm-1It is C-H to locate
Stretching vibration, 1734cm-1Locate the stretching vibration peak for C=O, 1144cm-1Locate the symmetrically flexible peak for C-O singly-bounds, 1005cm-1Locate to be the flexible peak of the antisymmetry of C-O singly-bounds, 1462cm-1Locate as-CH3The deformation vibration of middle C-H, 1381cm-1Locate as in=CH2
The deformation vibration of C-H, 771cm-1Locate as-CH2-CH2- carbon skeleton vibration peak, 1292cm-1Place is the C-H faces being connected with sulphur atom
Outer rocking vibration peak, 698cm-1It is C-S stretching vibration peaks to locate.Meanwhile, in 2560cm-1Left and right is illustrated in the change without absworption peak
Do not exist S-H keys in compound, just say that the hydrogen atom that antimony atoms instead of in S-H keys forms Sb-S keys yet.
(2) preparation of single-ethylhexyl maleate antimony：
10.29g (0.105mol) maleic anhydrides and 13.00g (0.1mol) isooctanol, magnetic force is added to stir in round-bottomed flask
Mix, 95 DEG C of back flow reaction 6h, three days are stood after completion of the reaction, after unreacted maleic anhydride is fully precipitated, by recirculated water
Formula vacuum pump pressure is filtered, and reclaims filter residue maleic anhydride, collects filtrate, obtains single-ethylhexyl maleate.
Material molar ratio is pressed in round-bottomed flask for single-ethylhexyl maleate：Antimony acetate=3:1 adds horse obtained in the first step
Come sour mono octyl ester and antimony acetate, magnetic agitation, 125 DEG C of Depressor response 1h obtain oiliness antimony system color development ink and increase after completion of the reaction
Toner raw material ----liquid single-ethylhexyl maleate antimony YSb2, it is standby.
Bibliography：
The synthesis in water and its property of [1] Qian Danyi, Gao Erjin, Tang Wei, Chen Si, Wang Xu five (isooctyl thioglycolate) antimony
Can research [J] plastics industries, 2010,10:70-73.
[2] research [D] the Central South University of the synthesis of Liu Yan five (isooctyl thioglycolate) antimony and its thermal stability,
2002.
[3] Liu Younian, Xun Yujun, Liu Yan, relax ten thousand blunt .PVC heat stabilizers five (isooctyl thioglycolate) antimony synthesis and
Its property [J] Zhongnan Polytechnic Univ's journal (natural science edition), 2002,06:588-591.
The preparation of the oiliness titanium system color development ink toner raw material of embodiment 2
(1) tetraisopropyl titanate and 288g (2mol) isooctyl acid of 284g (1mol), room temperature electricity are added in round-bottomed flask
Dynamic stirring 1 hour, 100 DEG C of back flow reaction 2h are removed under reduced pressure small molecule after completion of the reaction, cooling, obtain thick liquid isooctyl acid
Titanium isopropoxy compound ((C3H7O)mTi(OOCC7H15)n), this is oiliness titanium system color development ink toner raw material YT1, standby
With.
(2) butyl titanate and 432g (3mol) isooctyl acid of 340g (1mol) are added in round-bottomed flask, room temperature is electronic
Stirring 1 hour, 140 DEG C of back flow reaction 2h are removed under reduced pressure small molecule after completion of the reaction, cooling, obtain thick liquid isooctyl acid titanium
Butoxy compound ((C4H9O)mTi(OOCC7H15)n), this is oiliness titanium system color development ink toner raw material YT2, standby.
Embodiment 3-8 is that the toner raw material prepared using embodiment 1 and 2 is prepared oiliness ceramics to ooze colored color development ink hyperchromic
Agent.
Embodiment 3
At room temperature be well mixed for 93 mass parts YSb1 and 7 mass parts isooctyl acids and obtain final product 100 mass parts by the ratio according to table 1
Oiliness ceramics ooze colored color development ink toner, and it is 5 to measure its pH value.Then its 5 mass parts is taken, with the matter of yellow color development ink 100
After amount part is well mixed at room temperature, filtered by 0.3 μm of filter opening, filtrate and gilvous color development ink are sprayed by numeral respectively
Ink is printed upon in ceramic body or glaze paint, and by high temperature, 650 DEG C are burnt till 4 hours, and the increasing of ceramic body or glaze paint is observed after cooling
Ink hair color effect before and after color.Experimental result is listed in Table 1 below last 1 row.
Embodiment 4
Ratio according to table 1 mixes 5 mass parts YSb2,45 mass parts YT1 and 50 mass parts isooctyl acid butyl esters at room temperature
Uniformly obtaining final product 100 mass parts oiliness ceramics oozes colored color development ink toner, and it is 7 to measure its pH value.Then its 45 mass parts is taken, with
After the mass parts of yellow color development ink 100 are well mixed at room temperature, filtered by 5 μm of filter openings, by filtrate and gilvous color development ink
Water is printed upon on ceramic body or glaze paint by digital ink-jet respectively, and by high temperature, 800 DEG C are burnt till 3 hours, and pottery is observed after cooling
The hyperchromic front and rear ink hair color effect of porcelain base substrate or glaze paint.Experimental result is listed in Table 1 below last 1 row.
Embodiment 5
According to the ratio of table 1 by 2 mass parts YSb1,5 mass parts zinc Isoocatanoates, 53 mass parts YT2 and 40 mass parts methyl
Isooctyl acrylate monomer is well mixed and obtains final product 100 mass parts oiliness ceramics and ooze colored color development ink toner at room temperature, measures its pH value
It is 6.Then its 20 mass parts is taken, after being well mixed at room temperature with the mass parts of yellow color development ink 100, by 0.8 μm of filter opening
Filtering, filtrate and gilvous color development ink is printed upon on ceramic body or glaze paint by digital ink-jet respectively, by high temperature
1000 DEG C are burnt till 2 hours, and the hyperchromic front and rear ink hair color effect of ceramic body or glaze paint is observed after cooling.Experimental result is listed in table
Last 1 row in 1.
Embodiment 6
According to the ratio of table 1 by 40 mass parts zirconium iso-octoates, 20 mass parts YSb2 and 10 mass parts isooctyl acids, 30 mass parts
C7~C15Alkane is well mixed and obtains final product 100 mass parts oiliness ceramics and ooze colored color development ink toner at room temperature, and measuring its pH value is
5.Then its 30 mass parts is taken, after being well mixed at room temperature with the mass parts of yellow color development ink 100, by 0.5 μm of filter opening mistake
Filter, filtrate and gilvous color development ink is printed upon on ceramic body or glaze paint by digital ink-jet respectively, by high temperature 1200
DEG C burn till 1.5 hours, observed after cooling ceramic body or glaze paint it is hyperchromic before and after ink hair color effect.Experimental result is listed in table 1
In it is last 1 row.
Embodiment 7
According to the ratio of table 1 by 10 mass parts zinc Isoocatanoates, 20 mass parts zirconium iso-octoates and 40 mass parts stannous iso caprylates
It is well mixed at room temperature with 10 mass parts isooctyl acids, 20 mass parts Isooctyl acrylate monomers and obtains final product 100 mass parts oiliness ceramics and ooze flower
Color development ink toner, it is 4 to measure its pH value.Then its 10 mass parts is taken, is mixed at room temperature with the mass parts of yellow color development ink 100
After closing uniformly, filtered by 3 μm of filter openings, filtrate is printed upon ceramic blank by digital ink-jet respectively with pure red color development ink
On body or glaze paint, by high temperature, 1250 DEG C are burnt till 1 hour, and the hyperchromic front and rear ink color development of ceramic body or glaze paint is observed after cooling
Effect.Experimental result is listed in Table 1 below last 1 row.
Embodiment 8
According to the ratio of table 1 by 20 mass parts zirconium iso-octoates, 40 mass parts dibutyl tin laurates and 30 mass parts C10
~C20Alkane, 10 mass parts isooctyl acids are well mixed and obtain final product 100 mass parts oiliness ceramics and ooze colored color development ink toner at room temperature,
It is 5 to measure its pH value.Then its 45 mass parts is taken, after being well mixed at room temperature with the mass parts of yellow color development ink 100, by 1 μ
The filter opening filtering of m, filtrate is printed upon on ceramic body or glaze paint by digital ink-jet respectively with pure red color development ink, is passed through
1250 DEG C of high temperature is burnt till 1 hour, and the hyperchromic front and rear ink hair color effect of ceramic body or glaze paint is observed after cooling.Experimental result is arranged
Last 1 row in table 1.
Table 1：The toner composition of embodiment 3~8, pH value, usage ratio and hyperchromic effect
Hyperchromic effect is and visually observes in table 1.
From the result of table 1, after oiliness toner prepared by the present invention is mixed with color development ink by proper proportion, can be significantly
Improve the vividness that original color development ink is in pattern.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (6)
1. a kind of oiliness ceramics ooze colored color development ink toner, it is characterised in that the toner is by the hyperchromic gold of 50~95wt%
The organic solvent composition of category compound and 50~5wt%, the hyperchromic metallic compound organises for antimony, titanium, zirconium, zinc and tin
At least one in compound；The organic solvent is at least one in acids solvent, varsol and esters solvent.
2. a kind of oiliness ceramics according to claim 1 ooze colored color development ink toner, it is characterised in that the hyperchromic gold
Category compound for antimony oxygen/sulphur ligand complex, the carboxylic acid alkoxide compound of titanium, the ethylhexanoate salt of zirconium, the ethylhexanoate salt of zinc,
Neodecanoate, at least one in the ethylhexanoate salt and dibutyl tin laurate of tin.
3. a kind of oiliness ceramics according to claim 2 ooze colored color development ink toner, it is characterised in that and described oxygen/
Sulphur part is including isooctyl acid, butyl maleate, Malaysia monooctyl acid monooctyl ester, fourth containing aerobic or element sulphur ligand compound
Two monooctyl acid monooctyl esters, the different monooctyl ester of adipic acid list, the different monooctyl ester of decanedioic acid list, O-phthalic monooctyl acid monooctyl ester or TGA are different pungent
Ester.
4. a kind of oiliness ceramics according to claim 1 ooze colored color development ink toner, it is characterised in that described is organic
Solvent is isooctyl acid, neodecanoic acid, C7~C20Liquid long chain alkane, tricaprylate, neodecanoic acid ester, long alkyl chain methacrylates and third
At least one in olefin(e) acid long-chain ester.
5. the oiliness ceramics described in any one of Claims 1-4 ooze the preparation method of colored color development ink toner, and its feature exists
In comprising the following steps：Hyperchromic metallic compound is well mixed with organic solvent at room temperature, that is, it is 4~7 to obtain pH value
Oiliness ceramics ooze colored color development ink toner.
6. the oiliness ceramics described in any one of Claims 1-4 ooze the application method of colored color development ink toner, and its feature exists
In comprising the following steps：
(1) oiliness ceramics are oozed into colored color development ink toner with oiliness color development ink by 4~50:100 mass ratio is mixed at room temperature
Close uniform, filtered by less than 5 μm of filter openings, gained filtrate is printed upon on ceramic body or base substrate glaze surface through digital ink-jet；
(2) high temperature for being dried with 650~1250 DEG C by infiltration again burns till 1~4 hour, color development ink stabilization is manifested various fresh
Gorgeous pattern.
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| CN201611243299.9A CN106752376B (en) | 2016-12-29 | 2016-12-29 | Oil-based ceramic bleeding color development ink toner and preparation and use method thereof |
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| CN201611243299.9A CN106752376B (en) | 2016-12-29 | 2016-12-29 | Oil-based ceramic bleeding color development ink toner and preparation and use method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108929592A (en) * | 2018-08-06 | 2018-12-04 | 佛山科学技术学院 | A kind of white infiltration caul-fat ink and preparation method thereof for ceramic ink jet printing |
| CN115594791A (en) * | 2022-10-20 | 2023-01-13 | 广州聚佳新材料科技有限公司（Cn） | Solvent-free acrylic resin and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1420916A (en) * | 2000-01-07 | 2003-05-28 | 费罗公司 | Individual inks and ink set for use in color ink jet printing of glazed ceramic tiles and surfaces |
-
2016
- 2016-12-29 CN CN201611243299.9A patent/CN106752376B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1420916A (en) * | 2000-01-07 | 2003-05-28 | 费罗公司 | Individual inks and ink set for use in color ink jet printing of glazed ceramic tiles and surfaces |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108929592A (en) * | 2018-08-06 | 2018-12-04 | 佛山科学技术学院 | A kind of white infiltration caul-fat ink and preparation method thereof for ceramic ink jet printing |
| CN115594791A (en) * | 2022-10-20 | 2023-01-13 | 广州聚佳新材料科技有限公司（Cn） | Solvent-free acrylic resin and preparation method and application thereof |
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| CN106752376B (en) | 2020-08-07 |
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Effective date of registration: 20220927 Address after: 512400 No.3 complex building, Ping'an 1st Road, Dongguan Dalingshan (Nanxiong) industrial transfer industrial park, Nanxiong City, Shaoguan City, Guangdong Province Patentee after: Guoke Guanghua (Nanxiong) New Materials Research Institute Co.,Ltd. Patentee after: GUANGZHOU CHEMISTRY Co.,Ltd. CHINESE ACADEMY OF SCIENCES Address before: 512400 Zhuji Industrial Park, Nanxiong City, Shaoguan City, Guangdong Province (Nanxiong Fine Chemical Base, Guangdong Province) Patentee before: NANXIONG MATERIAL PRODUCTION BASE OF CHINESE ACADEMY OF SCIENCES GUANGZHOU CHEMICAL Co.,Ltd. Patentee before: GUANGZHOU CHEMISTRY Co.,Ltd. CHINESE ACADEMY OF SCIENCES |