CN116396636A - Black pigment for ceramic ink-jet printing and preparation method and application thereof - Google Patents
Black pigment for ceramic ink-jet printing and preparation method and application thereof Download PDFInfo
- Publication number
- CN116396636A CN116396636A CN202310352230.3A CN202310352230A CN116396636A CN 116396636 A CN116396636 A CN 116396636A CN 202310352230 A CN202310352230 A CN 202310352230A CN 116396636 A CN116396636 A CN 116396636A
- Authority
- CN
- China
- Prior art keywords
- ceramic
- sio
- black
- pigment
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 115
- 239000000049 pigment Substances 0.000 title claims abstract description 101
- 238000007641 inkjet printing Methods 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 73
- 239000000463 material Substances 0.000 claims abstract description 37
- 239000002994 raw material Substances 0.000 claims abstract description 31
- 238000010304 firing Methods 0.000 claims abstract description 27
- 239000002243 precursor Substances 0.000 claims abstract description 27
- 150000003839 salts Chemical class 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 229910020599 Co 3 O 4 Inorganic materials 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 77
- 239000000243 solution Substances 0.000 claims description 70
- 239000000047 product Substances 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 33
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 28
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 23
- 238000004040 coloring Methods 0.000 claims description 23
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical group O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000000084 colloidal system Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003086 colorant Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 239000003929 acidic solution Substances 0.000 claims description 5
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims description 2
- 150000004690 nonahydrates Chemical group 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 238000011161 development Methods 0.000 abstract description 13
- 230000007547 defect Effects 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 32
- 239000000976 ink Substances 0.000 description 32
- 239000011435 rock Substances 0.000 description 11
- 241000519995 Stachys sylvatica Species 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000005498 polishing Methods 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 229960000583 acetic acid Drugs 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000012362 glacial acetic acid Substances 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 229910020630 Co Ni Inorganic materials 0.000 description 2
- 229910002440 Co–Ni Inorganic materials 0.000 description 2
- 206010027627 Miliaria Diseases 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 201000004169 miliaria rubra Diseases 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910003321 CoFe Inorganic materials 0.000 description 1
- 229910000684 Cobalt-chrome Inorganic materials 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 241001448624 Miliaria Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000010952 cobalt-chrome Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000010020 roller printing Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000004018 waxing Methods 0.000 description 1
- 229940045860 white wax Drugs 0.000 description 1
Classifications
-
- 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
-
- 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
Abstract
The invention belongs to the technical field of ceramic pigment, and provides a black pigment for ceramic inkjet printing, a preparation method and application thereof, wherein the black pigment for ceramic inkjet printing comprises the following raw materials in proportion: 72-85 parts of pigment main body and 15-28 parts of special powder; the pigment main body is prepared by mixing and firing the following raw materials: 16-24 parts of Cr 2 O 3 10-14 parts of Fe 2 O 3 26-34 parts of Co 3 O 4 And 14-17 parts of NiO; the special powder is made of SiO-containing material 2 The organosilicon source and the water-soluble ferric salt are used as precursors, and the SiO is formed by the reaction and calcination of an acid solution 2 With Fe 2 O 3 The mass ratio of the powder is 1.0-1.5. The black pigment for ceramic ink-jet printing is obtained by the cooperation of the pigment main body and the special powder, so that the obtained black ceramic ink-jet printing ink has more pure black color development performance, especially on the full-polished ceramic product, and basically does not generateWhite spots or glaze defects.
Description
Technical Field
The invention relates to the technical field of ceramic pigments, in particular to a black pigment for ceramic ink-jet printing, a preparation method and application thereof.
Background
Ceramic inkjet printing technology has been developed for decades, and has completely replaced the traditional roller and screen printing technology, and the product types have gradually developed into glazed tiles, archaized tiles and rock plates. In recent years, the rise of rock plates has placed higher demands on ceramic colorants and ceramic inks. According to trend of ceramic building industry in recent two and three years, dark ceramic tile products are more and more, and the design style of the dark ceramic tile is widely used for all-polished glaze, archaized tiles and ceramic rock plate products, so that the use amount of black ink is increased.
The existing black pigment, as shown in the cobalt black pigment for ceramic ink and the preparation method thereof provided in publication No. CN108456450B, is prepared from a pigment such as Cr 2 O 3 、Fe 2 O 3 、Co 3 O 4 、NiO、MnO 2 The main raw materials of the (C) are directly and uniformly mixed in proportion and then are subjected to solid-phase firing at high temperature; the preparation method is mature and simple, and is widely used.
However, when the existing black ceramic ink-jet printing ink prepared from the black pigment changes in the glaze formula, firing temperature and other processes of ceramic products, the black pigment in the black ceramic ink-jet printing ink is easy to react with ceramic glaze in the firing process of ceramic products (such as glaze polishing), so that the black ceramic ink-jet printing ink is easy to generate unstable and impure color, a large number of bubbles are easy to form at the printing ink, and some bubbles cannot be timely discharged, so that closed air holes are easy to form under the glaze polishing products, and are exposed after fine polishing by a polishing machine to become open air holes, and white wax is filled in the open air holes after the waxing process, so that the surface of the polished glaze polishing product finally forms macroscopic white spots (namely tiny white pinholes), thereby seriously affecting the attractive appearance, antifouling property and high-grade rate of the ceramic products.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a black pigment for ceramic ink-jet printing, a preparation method and application thereof, so that the black ceramic ink-jet printing ink obtained by using the black pigment has more pure black color development performance on ceramic products (especially full polished ceramic products) and basically does not generate white spots or glaze defects.
Based on the above, the invention discloses a black pigment for ceramic ink-jet printing, which comprises the following raw materials in parts by mass:
72-85 parts of pigment main body
15-28 parts of special powder;
wherein the pigment main body is prepared by mixing and firing the following raw materials in parts by mass:
wherein the special powder is prepared from a powder containing SiO 2 The organosilicon source and the water-soluble ferric salt are used as precursors, and are sequentially reacted by acid solution and calcined to form the SiO-containing material 2 And Fe (Fe) 2 O 3 Is a powder of (1); and SiO in the special powder 2 With Fe 2 O 3 The mass ratio of (2) is 1.0-1.5.
Preferably, the pH of the acidic solution is less than or equal to 4.0.
Further preferably, siO in the special powder 2 With Fe 2 O 3 The mass ratio of (2) was 1.25.
Still more preferably, the black pigment for ceramic inkjet printing comprises the following raw materials in parts by mass:
78 parts of pigment main body
22 parts of special powder;
wherein, the pigment main body comprises the following raw materials in parts by mass:
preferably, the SiO-containing layer 2 The organosilicon source of (C) is SiO-containing 2 Ethyl orthosilicate of (2), siO in said ethyl orthosilicate 2 The mass content of (2) is 20-40%.
Wherein for SiO-containing materials such as water glass, silica sol, etc 2 Tests show that in the process of preparing the special powder, the liquid-phase inorganic silicon source is hard to carry out subsequent operation due to drying and hardening, so the special powder cannot be prepared by using the liquid-phase inorganic silicon source. In addition, siO-containing materials such as quartz powder 2 The solid inorganic silicon source has large particles and low activity, and is difficult to react with an acid solution to form dark brown colloid together with water-soluble ferric salt, so that the effect of a liquid phase method is difficult to achieve.
Therefore, the invention adopts the SiO-containing material 2 Organosilicon sources (e.g. containing SiO) 2 Silicate esters of (a) preferably SiO-containing 2 Tetraethoxysilane (SiO thereof) 2 The mass content of (a) is 20-40%) is used as one of the precursors, and the precursor reacts under an acidic solution, so that a dark brown colloid is formed together with the other precursor (water-soluble ferric salt), and then the special powder with high quality and high yield is obtained by calcination.
Preferably, the water-soluble ferric salt is ferric nitrate nonahydrate.
Wherein, for example, fe 2 O 3 Such water-insoluble solid iron source is hardly reacted with the acidic solution because of large particles and low activity 2 The organic silicon sources of (2) together form dark brown colloid, so that the effect of a liquid phase method is difficult to achieveAnd (5) fruits. The content and the types of byproducts formed by different water-soluble ferric salts are different, so that the quality of the special powder is affected to a certain extent. The water-soluble iron salt of the present invention is therefore preferably ferric nitrate nonahydrate.
The invention also discloses a preparation method of the black pigment for ceramic ink-jet printing, which comprises the following steps:
s1, preparing special powder:
s11, preparing SiO-containing materials 2 An alcoholic solution of a silicone source and an aqueous solution of a water-soluble ferric salt;
s12, slowly dripping the water solution of the water-soluble ferric salt into the SiO-containing solution while stirring 2 Obtaining a mixed solution in an alcohol solution of an organosilicon source;
s13, placing the mixed solution in a constant-temperature water bath at 80-100 ℃, slowly dropwise adding an acid solution into the mixed solution under continuous stirring until the pH value is less than or equal to 4.0 to obtain a dark brown solution, and continuously stirring to obtain a dark brown colloid;
s14, drying the dark brown colloid, and calcining at 1150-1180 ℃ for 3-4h to obtain SiO 2 With Fe 2 O 3 The mass ratio of the powder is 1.0 to 1.5;
s2, preparing a pigment main body: according to the proportion of raw materials, respectively weighing Cr 2 O 3 、Fe 2 O 3 、Co 3 O 4 And NiO, stirring uniformly, firing at 1160-1220 ℃ for 5-8h, grinding until the fineness is less than or equal to 325 meshes, and obtaining a pigment main body;
s3, preparing a black pigment: mixing the special powder and the pigment main body according to the raw material proportion, and homogenizing to obtain the black pigment for ceramic inkjet printing.
Preferably, in the step S11, the SiO-containing layer is formed 2 The organic silicon source alcohol solution is SiO-containing 2 The preparation process of the tetraethoxysilane alcohol solution comprises the following steps: will contain 20-40% SiO 2 Dissolving ethyl orthosilicate in absolute ethanol, and stirring uniformly to obtain SiO-containing solution 2 Ethyl orthosilicate alcohol solution;
the water solution of the water-soluble ferric salt is a nonahydrate ferric nitrate water solution, and the preparation process comprises the following steps: and dissolving ferric nitrate nonahydrate in distilled water, and uniformly stirring to obtain the ferric nitrate nonahydrate solution.
Wherein, the mass conversion relation between the tetraethoxysilane and the ferric nitrate nonahydrate in the step S1 is as follows:
let m (ethyl orthosilicate) =a, m (ferric nitrate nonahydrate) =b, and let m (SiO) in the powder body 2 ):m(Fe 2 O 3 ) For example, =1.25, siO of tetraethyl orthosilicate 2 The mass content is 40% by weight, the m (SiO 2 ) 0.4A;
then m (SiO) 2 )＝1.25·m(Fe 2 O 3 ) This can be done in turn by the following equations (1) to (5):
0.4A＝1.25·M(Fe 2 O 3 )·n(Fe 2 O 3 ) (1)
0.4A＝1.25·M(Fe 2 O 3 )·n(Fe 3+ )/2 (2)
0.4A＝1.25·M(Fe 2 O 3 ) N (ferric nitrate nonahydrate)/2 (3)
0.8A＝1.25·M(Fe 2 O 3 ) M (ferric nitrate nonahydrate)/M (ferric nitrate nonahydrate) (4)
0.8a·m (ferric nitrate nonahydrate) =1.25·m (Fe) 2 O 3 )·B (5)
Wherein M (ferric nitrate nonahydrate) =404 g/mol, M (Fe) 2 O 3 )＝160g/mol；
Thus, the above-mentioned conversion formula (5) can be converted to: a=0.619B.
In step S13, the SiO-containing layer 2 Under the heating condition of constant-temperature water bath, the tetraethoxysilane in the tetraethoxysilane alcohol solution is hydrolyzed to generate silicic acid and ethanol, and along with the progress of hydrolysis reaction, the temperature of a mixed solution system is increased, and the ethanol and water in the mixed solution system gradually volatilize, so that silicic acid molecules wrap Fe 3+ The colloidal structure of the ion (i.e., dark brown colloid). The dark brown colloid forms SiO at high temperature during the calcination in step S14 2 And Fe (Fe) 2 O 3 And then cool downObtaining special powder.
The applicant has found that, in the preparation of black pigments, if Fe 2 O 3 Are all directly added into Cr-Fe-Co-Ni system (i.e. Fe 2 O 3 Directly with Cr 2 O 3 、Co 3 O 4 NiO and SiO 2 Mixing, grinding and firing into black pigment), the black color development performance (such as shiny color and reddish tone) of the black ceramic ink-jet printing ink prepared by the black pigment on ceramic products (especially full-polished ceramic products) can be affected, and the glaze defect (the number of white spots on the surfaces of the full-polished ceramic products is obviously increased or prickly heat exists on the glaze of the rock board ceramic products) of the black ceramic ink-jet printing ink on the ceramic products (such as the full-polished ceramic products and the rock board ceramic products) can be increased.
Thus, the present invention prepares a specific powder (which is prepared by using a powder containing SiO 2 The organosilicon source and the water-soluble ferric salt are used as precursors, and are sequentially reacted by acid solution and calcined to form SiO 2 With Fe 2 O 3 Powder with a mass ratio of 1.0-1.5), and then preparing the pigment main body (namely, part of Fe 2 O 3 Directly added to Cr 2 O 3 、Co 3 O 4 And NiO, firing and grinding to obtain the product; finally, mixing the special powder with the pigment main body to prepare a black pigment; thus, the special powder and the pigment main body are prepared in two steps respectively, and Fe can be effectively avoided 2 O 3 With Cr 2 O 3 、Co 3 O 4 NiO forms various mixed crystal forms, so that the Cr-Fe-Co-Ni system basically forms CoCr 2 O 4 、NiFe 2 O 4 Reducing e.g. Fe 2 Cr 2 O 4 、CoFe 2 O 4 The crystal structure which is easy to react with the ceramic glaze is used for improving the stability of the ceramic glaze and the ink in the ceramic firing process, avoiding the adverse effect of various mixed crystal forms and the ceramic glaze on the absorption and refraction of light, further improving the color development stability of the ink prepared by the black pigment on ceramic products (especially full-polished ceramic products), and reducing the glaze defects (such as white points, miliaria and the like) of the ink on the ceramic products.
The invention also discloses an application of the black pigment for ceramic ink-jet printing, which comprises the following steps: grinding and dispersing black pigment for ceramic ink-jet printing to obtain the final product with solid content of 35-45wt.% and particle size D 50 Black ceramic inkjet printing ink of 0.3-0.4 μm; and then the black ceramic ink-jet printing ink is ink-jet printed on the glaze of the ceramic, so as to obtain the ceramic product by firing.
In practice, the black pigment is ground and dispersed to prepare black ceramic ink-jet printing ink; this process is prior art and will not be described in detail.
Preferably, the black ceramic ink-jet printing ink is ink-jet printed on the glaze of the full-polished ceramic, so as to obtain the full-polished ceramic product by firing.
Compared with the prior art, the invention at least comprises the following beneficial effects:
the invention adds part of Fe 2 O 3 Directly added to Cr 2 O 3 、Co 3 O 4 And NiO to fire the colour former body; and contains SiO 2 The organosilicon source and the water-soluble ferric salt are used as precursors, and the special powder is formed by acid solution reaction and calcination in sequence, and the SiO in the special powder is controlled 2 With Fe 2 O 3 The mass ratio of (2) is 1.0-1.5; thus, the black pigment for ceramic ink-jet printing is obtained by matching the pigment main body with the special powder, so that the black ceramic ink-jet printing ink prepared by adopting the black pigment can show more pure black color development performance on ceramic products (especially full polished ceramic products), white spots or glaze defects can not be generated basically, and the comprehensive performance is good.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof.
Example 1
The black pigment for ceramic ink-jet printing comprises the following raw materials in parts by mass:
78 parts of pigment main body
22 parts of special powder;
wherein the pigment main body is prepared by mixing and firing the following raw materials in parts by mass:
wherein the special powder contains SiO 2 The organosilicon source and the water-soluble ferric salt are used as precursors, and the SiO-containing material is formed by sequentially carrying out acid solution reaction and calcination 2 And Fe (Fe) 2 O 3 Is a powder of (1); and SiO in the special powder 2 With Fe 2 O 3 The mass ratio of (2) was 1.25. Therefore, the black coloring material of this example was produced by tailoring SiO in powder in terms of parts by mass 2 12.2 parts of Fe 2 O 3 9.8 parts.
The preparation method of the black pigment for ceramic ink-jet printing comprises the following steps:
s1, preparing special powder:
s11, weighing 225g of tetraethoxysilane (SiO thereof) 2 The mass content of (2) is 40 percent) is dissolved in 250mL absolute ethyl alcohol and is stirred uniformly to obtain solution A; 363.6g of ferric nitrate nonahydrate is weighed and dissolved in 242g of distilled water, and the solution B is obtained by stirring uniformly;
s12, slowly dripping the solution B into the solution A while stirring, magnetically stirring for 25min, and uniformly mixing to obtain a solution C;
s13, carrying out constant-temperature water bath on the solution C at 80 ℃, continuously stirring, slowly dropwise adding 0.1mol/L glacial acetic acid solution into the solution C until the pH value is=3.8, and continuously stirring for 45min to obtain a dark brown colloid (namely a special precursor);
s14, placing the special precursor into a 180 ℃ oven for drying, placing the special precursor into a muffle furnace, and calcining the special precursor for 4 hours at 1160 ℃ to obtain special powder, wherein m (SiO 2 ):m(Fe 2 O 3 )＝1.25。
S2, preparing a pigment main body: press onThe raw materials are proportioned and Cr is respectively weighed 2 O 3 、Fe 2 O 3 、Co 3 O 4 And NiO, placing in a mixer, stirring uniformly, placing in a tunnel kiln, firing at 1190deg.C for 6h to obtain pigment, processing the pigment by a powdering machine until the fineness is 325 mesh full-pass or smaller, and bagging.
S3, preparing a black pigment: and (3) mixing the special powder in the step (S1) and the pigment main body in the step (S2) according to the raw material ratio, and homogenizing for 30min to obtain the black pigment for ceramic inkjet printing.
Example 2
The black pigment for ceramic ink-jet printing comprises the following raw materials in parts by mass:
85 parts of pigment main body
15 parts of special powder;
wherein the pigment main body is prepared by mixing and firing the following raw materials in parts by mass:
wherein the special powder contains SiO 2 The organosilicon source and the water-soluble ferric salt are used as precursors, and are sequentially reacted by acid solution and calcined to form the SiO-containing material 2 And Fe (Fe) 2 O 3 Is a powder of (1); siO in the special powder 2 With Fe 2 O 3 The mass ratio of (2) was 1.0.
The preparation method of the black pigment for ceramic ink-jet printing comprises the following steps:
s1, preparing special powder:
s11, weighing 225g of tetraethoxysilane (SiO thereof) 2 The mass content of (2) is 40 percent) is dissolved in 250mL absolute ethyl alcohol and is stirred uniformly to obtain solution A; 454.5g of ferric nitrate nonahydrate is weighed and dissolved in 303g of distilled water, and the solution B is obtained by stirring uniformly;
s12, slowly dripping the solution B into the solution A while stirring, magnetically stirring for 25min, and uniformly mixing to obtain a solution C;
s13, carrying out constant-temperature water bath on the solution C at 80 ℃, continuously stirring, slowly dropwise adding 0.1mol/L glacial acetic acid solution into the solution C until the pH value is=3.9, continuously stirring for 45min to obtain a dark brown solution, and obtaining a dark brown colloid (namely a special precursor);
s14, putting the special precursor into a 180 ℃ oven for drying, putting the special precursor into a muffle furnace, and calcining the special precursor for 3 hours at 1150 ℃ to obtain special powder, wherein m (SiO 2 ):m(Fe 2 O 3 )＝1.0。
S2, preparing a pigment main body: weighing Cr according to the proportion of the raw materials 2 O 3 、Fe 2 O 3 、Co 3 O 4 And NiO, placing the mixture into a mixer for uniform stirring, placing the mixture into a tunnel kiln for firing for 5 hours at 1160 ℃ to obtain pigment, processing the pigment by a powdering machine until the fineness is 325 meshes or less, obtaining a pigment main body, and bagging for later use.
S3, preparing a black pigment: and (3) mixing the special powder in the step (S1) and the pigment main body in the step (S2) according to the raw material ratio, and homogenizing for 30min to obtain the black pigment for ceramic inkjet printing.
Example 3
The black pigment for ceramic ink-jet printing comprises the following raw materials in parts by mass:
72 parts of pigment main body
28 parts of special powder;
wherein the pigment main body is prepared by mixing and firing the following raw materials in parts by mass:
wherein the special powder contains SiO 2 The organosilicon source and the water-soluble ferric salt are used as precursors, and the following steps are sequentially carried outThrough acidic solution reaction and calcination, the SiO-containing material is formed 2 And Fe (Fe) 2 O 3 Is a powder of (1); siO in the special powder 2 With Fe 2 O 3 The mass ratio of (2) was 1.5.
The preparation method of the black pigment for ceramic ink-jet printing comprises the following steps:
s1, preparing special powder:
s11, weighing 225g of tetraethoxysilane (SiO thereof) 2 The mass content of (2) is 40 percent) is dissolved in 250mL absolute ethyl alcohol and is stirred uniformly to obtain solution A; 303g of ferric nitrate nonahydrate is weighed and dissolved in 202g of distilled water, and the solution B is obtained after uniform stirring;
s12, slowly dripping the solution B into the solution A while stirring, magnetically stirring for 25min, and uniformly mixing to obtain a solution C;
s13, carrying out constant-temperature water bath on the solution C at 80 ℃, continuously stirring, slowly dropwise adding 0.1mol/L glacial acetic acid solution into the solution C until the pH value is=3.6, and continuously stirring for 45min to obtain a dark brown colloid (namely a special precursor);
s14, putting the special precursor into a 180 ℃ oven for drying, putting the special precursor into a muffle furnace, and calcining the special precursor for 4 hours at 1180 ℃ to obtain special powder, wherein m (SiO 2 ):m(Fe 2 O 3 )＝1.5。
S2, preparing a pigment main body: weighing Cr according to the proportion of the raw materials 2 O 3 、Fe 2 O 3 、Co 3 O 4 And NiO, placing the mixture into a mixer for uniform stirring, placing the mixture into a tunnel kiln for firing for 7 hours at 1220 ℃ to obtain a pigment, processing the pigment by a powdering machine until the fineness is 325 meshes or less, obtaining a pigment main body, and bagging for later use.
S3, preparing a black pigment: and (3) mixing the special powder in the step (S1) and the pigment main body in the step (S2) according to the raw material ratio, and homogenizing for 30min to obtain the black pigment for ceramic inkjet printing.
Example 4
In this example, reference is made to example 1 for a black coloring material for ceramic inkjet printing and a method for producing the same, and the difference from example 1 is that:
in step S11 of this example, 281g of ethyl orthosilicate (SiO thereof) was weighed out at the time of preparing the solution A 2 Is 32% by mass).
In step S13 of this example, the pH of solution c=3.7 when preparing the specific precursor.
Example 5
In this example, reference is made to example 1 for a black coloring material for ceramic inkjet printing and a method for producing the same, and the difference from example 1 is that:
in step S11 of this example, 346g of ethyl orthosilicate (SiO thereof) was weighed out at the time of preparing the solution A 2 26% by mass).
Comparative example 1
A black coloring material of this comparative example and a method for producing the same are described in example 1, which differs from example 1 in that:
in the black coloring material of the comparative example, m (SiO 2 ):m(Fe 2 O 3 ) =1.7 (i.e. SiO in the tailored powder in parts by mass 2 Still 12.2 parts of Fe 2 O 3 Down to 7.2 parts).
Meanwhile, to ensure that Fe is directly added to the black coloring material of this comparative example (i.e., added in such a manner as to be added to the coloring material main body) 2 O 3 And indirectly (i.e. by adding in the form of special powder) Fe 2 O 3 The sum of parts by mass of (C) is the same as in example 1, and Fe is directly added to the coloring material main body in the black coloring material of this comparative example 2 O 3 The mass fraction of (2) is increased to 12.6 parts. The mass parts of the rest raw materials are unchanged.
Correspondingly, to prepare m (SiO 2 ):m(Fe 2 O 3 ) Special powder=1.7, in step S11 of this comparative example, the procedure for preparing solution B is: 267.7g of ferric nitrate nonahydrate is weighed and dissolved in 178g of distilled water, and the solution B is obtained by stirring uniformly. The rest steps are unchanged.
Comparative example 2
A black coloring material of this comparative example and a method for producing the same are described in example 1, which differs from example 1 in that:
10 parts of Fe directly added to the black coloring material of example 1 (i.e., added so as to be added to the main body of the coloring material) 2 O 3 All of Fe being indirectly added (i.e. added by means of special powder) 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the In this case, in the black coloring material of the comparative example, m (SiO 2 ):m(Fe 2 O 3 ) =0.62 (the specific powder still contains 12.2 parts of SiO 2 And Fe (Fe) 2 O 3 To 19.8 parts). The mass parts of the rest raw materials are unchanged.
Comparative example 3
A black coloring material of this comparative example and a method for producing the same are described in example 1, which differs from example 1 in that:
in step S13 of this comparative example, the pH of the solution C was=4.5, a brown solution was obtained, and no significant colloid was generated after stirring was continued for 45 minutes. The rest steps are unchanged.
Comparative example 4
The black pigment of the comparative example comprises the following raw materials in parts by mass:
that is, the black coloring material of this comparative example was omitted by 22 parts of the special powder as compared with example 1.
The preparation method of the black pigment of the comparative example comprises the following preparation processes: cr is weighed according to the proportion of the raw materials 2 O 3 、Fe 2 O 3 、Co 3 O 4 NiO and SiO 2 Placing the mixture in a mixer, uniformly stirring, placing the mixture in a tunnel kiln, firing the mixture at 1190 ℃ for 6 hours to obtain pigment, and processing the fired pigment by a powdering machine until the fineness is 325 meshes full-pass or smaller, thus obtaining the black pigment of the comparative example.
Performance testing
1. The preparation method of the black ceramic ink-jet printing ink comprises the following steps:
the black materials obtained in examples 1 to 5 and comparative examples 1 to 4 were prepared to have a solid content of 35 to 45 wt% and a particle size D by a grinding dispersion method, respectively 50 Black ceramic inkjet printing ink of 0.3-0.4 μm.
2. Black ceramic inkjet printing inks (solids content 40wt.%, particle size D) of examples 1-5 and comparative examples 1-4 were used 50 0.3 μm) are respectively applied to the full-polished ceramic products for color development and polished white spot test; wherein, when preparing the full-polished ceramic product, the printing quantity of the black ceramic ink-jet printing ink is 6.6g/m 2 The firing temperature zone of the fully glazed ceramic product is 1175-1180 ℃ and the firing time is 42min. The test results are shown in table 1 below.
TABLE 1
From the test data of table 1, it can be seen that:
(1) As is clear from examples 1 and 4, the addition of the specific powder to the black coloring material has a remarkable effect on both the black color development performance and the white point number performance of the ink, and the addition of the specific powder (as in comparative example 4) does not significantly reduce the black color development performance and the white point number of the black coloring material as compared with example 1.
(2) As is clear from example 1 and comparative example 3, when preparing the special precursor in step S13, the pH of the solution C needs to be controlled to be less than or equal to 4.0, otherwise, as shown in comparative example 3, a dark brown colloid is difficult to form in step S13, and the number of white spots is significantly increased.
(3) As is clear from example 1 and comparative examples 1 to 2, m (SiO 2 ):m(Fe 2 O 3 ) The ratio of a and b is reduced (the value of a is reduced from 1.3 to 0.1, and the value of b is reduced from-0.3 to-1.6), and the change range of the values of a and b is larger. Although, toProportion 2 (m (SiO in the special powder) 2 ):m(Fe 2 O 3 ) The white point number of =0.62) is relatively small, but m (SiO 2 ):m(Fe 2 O 3 ) The reduction of the ratio is limited to the improvement of the white point number. In addition, m (SiO) 2 ):m(Fe 2 O 3 ) The effect of the reduction in the ratio of (A) on the black hue is more pronounced, for example, in example 1 and comparative example 2, when m (SiO 2 ):m(Fe 2 O 3 ) When the ratio of (a) was decreased from 1.25 in example 1 to 0.62 in comparative example 2, the hue changed from red-black tone of a=1.0 and b= -0.8 to blue-green tone of a=0.1 and b= -1.6, and at this time, the red tone was insufficient and the blue tone was obvious in comparative example 2, and the black color was not pure enough.
Furthermore, when tailoring m (SiO 2 ):m(Fe 2 O 3 ) At=1.7 (comparative example 1), the black color turns light, the hue is reddish yellow, and the number of white spots increases significantly.
Thus, m (SiO) in the special powder is controlled 2 ):m(Fe 2 O 3 ) The ratio (the ratio is controlled between 1 and 1.5) of the black ceramic ink-jet printing ink prepared by the black pigment disclosed by the invention can enable the black ceramic ink-jet printing ink to be more pure black and have fewer white points on a full-polished ceramic product.
(4) As is clear from examples 1, 4-5, when solution A is prepared in step S11, siO in tetraethyl orthosilicate 2 When the mass content of (2) is reduced, the dosage of the tetraethoxysilane is correspondingly increased, and the same SiO is maintained 2 The total amount of the pigment does not substantially affect the black color development and white point number of the black pigment.
3. Black ceramic inkjet printing inks (solids content 45wt.%, particle size D) of examples 1-5 and comparative examples 1-4 were used 50 0.4 μm) was applied to the rock laminate ceramic product, respectively, for color development and glaze testing; wherein, when preparing the rock plate ceramic product, the printing quantity of the black ceramic ink-jet printing ink is 7g/m 2 The firing temperature area of the rock plate ceramic product is 1185-1190 ℃ and the firing time is 52min. The test results are shown in table 2 below.
TABLE 2
Note that: in tables 1 to 2, L represents luminance, a represents a range from magenta to green, b represents a range from yellow to blue, and the ranges of a and b are from +127 to-128.
From the test data of table 2, it can be seen that:
(1) As is clear from examples 1 and 4, the black ceramic inkjet printing ink prepared from the black colorant resulted in significant glaze defects (in particular, glaze prickly heat) on the rock plate ceramic products without the addition of special powder.
(2) As is clear from example 1 and comparative example 3, when the specific precursor is prepared in step S13, if the ph=4.5 of the solution C, a dark brown colloid cannot be effectively formed, and further, the ink prepared from the black pigment may have a glaze defect.
(3) As is clear from example 1 and comparative examples 1-2, the ink produced by the black colorant has less fluctuation of overall black color development on the rock plate ceramic product than the full-polished ceramic product; however, it can be seen that m (SiO 2 ):m(Fe 2 O 3 ) The lower ratio (e.g., comparative example 2) or the higher ratio (e.g., comparative example 1) of the ratio (i.e., the ratio of the ratio (i) to the ratio (ii) affects the black color development of the ink obtained from the black coloring material, and the ratio (i) of m (SiO) 2 ):m(Fe 2 O 3 ) If the ratio of (2) is lower than 1.0, the black color becomes blue, the color is not pure, and m (SiO 2 ):m(Fe 2 O 3 ) Above 1.5, the black color turns red and yellow.
In summary, the black coloring material of the present invention is obtained by adding a part of Fe to the main coloring material (which is 2 O 3 Directly added to Cr 2 O 3 、Co 3 O 4 And NiO, through firing and grinding), adding special powder, and controlling m (SiO) 2 ):m(Fe 2 O 3 ) =1-1.5, and when preparing the tailored precursor in step S13, controlling the pH of the solution C to be less than or equal to 4.0, to effectively form a dark brown colloid; thus, the black pigment can be obtainedThe black ceramic ink-jet printing ink has more pure black color development performance on the full-polished ceramic products and the rock plate ceramic products, basically does not generate white spots or glaze defects, and has good comprehensive performance.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiment and all such alterations and modifications as fall within the scope of the embodiments of the invention.
The foregoing has outlined rather broadly the more detailed description of the invention in order that the detailed description of the invention that follows may be better understood, and in order that the present principles and embodiments may be better understood; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in accordance with the ideas of the present invention, the present description should not be construed as limiting the present invention in view of the above.
Claims (10)
1. The black pigment for ceramic ink-jet printing is characterized by comprising the following raw materials in parts by mass:
72-85 parts of pigment main body
15-28 parts of special powder;
wherein the pigment main body is prepared by mixing and firing the following raw materials in parts by mass:
Cr 2 O 3 16-24 parts
Fe 2 O 3 10-14 parts
Co 3 O 4 26-34 parts
14-17 parts of NiO;
wherein the special powder is prepared from a powder containing SiO 2 The organosilicon source and the water-soluble ferric salt are used as precursors, and are sequentially reacted by acid solution and calcined to form the SiO-containing material 2 And Fe (Fe) 2 O 3 Is a powder of (1); and SiO in the special powder 2 With Fe 2 O 3 The mass ratio of (2) is 1.0-1.5.
2. The black colorant for ceramic inkjet printing according to claim 1 wherein the pH value of the acidic solution is 4.0 or less.
3. The black colorant for ceramic inkjet printing according to claim 1 or 2, wherein SiO in the tailored powder 2 With Fe 2 O 3 The mass ratio of (2) was 1.25.
4. A black pigment for ceramic inkjet printing according to claim 3, wherein the raw materials are as follows in parts by mass:
78 parts of pigment main body
22 parts of special powder;
wherein, the pigment main body comprises the following raw materials in parts by mass:
5. the black coloring material for ceramic inkjet printing according to claim 1 wherein the SiO-containing material is a mixture of a plurality of pigments 2 The organosilicon source of (C) is SiO-containing 2 Ethyl orthosilicate of (2), siO in said ethyl orthosilicate 2 The mass content of (2) is 20-40%.
6. The black colorant for ceramic inkjet printing according to claim 1 wherein the water-soluble iron salt is ferric nitrate nonahydrate.
7. The method for producing a black coloring material for ceramic inkjet printing according to any one of claims 1 to 6, comprising the steps of:
s1, preparing special powder:
s11, preparing SiO-containing materials 2 An alcoholic solution of a silicone source and an aqueous solution of a water-soluble ferric salt;
s12, slowly dripping the water solution of the water-soluble ferric salt into the SiO-containing solution while stirring 2 Obtaining a mixed solution in an alcohol solution of an organosilicon source;
s13, placing the mixed solution in a constant-temperature water bath at 80-100 ℃, slowly dropwise adding an acid solution into the mixed solution under continuous stirring until the pH value is less than or equal to 4.0 to obtain a dark brown solution, and continuously stirring to obtain a dark brown colloid;
s14, drying the dark brown colloid, and calcining at 1150-1180 ℃ for 3-4h to obtain SiO 2 With Fe 2 O 3 The mass ratio of the powder is 1.0 to 1.5;
s2, preparing a pigment main body: according to the proportion of raw materials, respectively weighing Cr 2 O 3 、Fe 2 O 3 、Co 3 O 4 And NiO, stirring uniformly, firing at 1160-1220 ℃ for 5-8h, grinding until the fineness is less than or equal to 325 meshes, and obtaining a pigment main body;
s3, preparing a black pigment: mixing the special powder and the pigment main body according to the raw material proportion, and homogenizing to obtain the black pigment for ceramic inkjet printing.
8. The method for preparing a black coloring material for ceramic inkjet printing according to claim 7, wherein in step S11, the SiO-containing material is 2 The organic silicon source alcohol solution is SiO-containing 2 The preparation process of the tetraethoxysilane alcohol solution comprises the following steps: will contain 20-40% SiO 2 Dissolving ethyl orthosilicate in absolute ethanol, and stirring uniformly to obtain SiO-containing solution 2 Ethyl orthosilicate alcohol solution;
the water solution of the water-soluble ferric salt is a nonahydrate ferric nitrate water solution, and the preparation process comprises the following steps: and dissolving ferric nitrate nonahydrate in distilled water, and uniformly stirring to obtain the ferric nitrate nonahydrate solution.
9. A black for ceramic ink-jet printing according to any one of claims 1 to 6The application of the color pigment is characterized in that the application method comprises the following steps: grinding and dispersing black pigment for ceramic ink-jet printing to obtain the final product with solid content of 35-45wt.% and particle size D 50 Black ceramic inkjet printing ink of 0.3-0.4 μm; and then the black ceramic ink-jet printing ink is ink-jet printed on the glaze of the ceramic, so as to obtain the ceramic product by firing.
10. The use of a black pigment for ceramic inkjet printing according to claim 9 wherein the black ceramic inkjet printing ink is inkjet printed onto the glaze of the full-glazed ceramic to produce a full-glazed ceramic product by firing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310352230.3A CN116396636B (en) | 2023-04-04 | 2023-04-04 | Black pigment for ceramic ink-jet printing and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310352230.3A CN116396636B (en) | 2023-04-04 | 2023-04-04 | Black pigment for ceramic ink-jet printing and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116396636A true CN116396636A (en) | 2023-07-07 |
| CN116396636B CN116396636B (en) | 2023-11-14 |
Family
ID=87006969
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310352230.3A Active CN116396636B (en) | 2023-04-04 | 2023-04-04 | Black pigment for ceramic ink-jet printing and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116396636B (en) |
Citations (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005054381A1 (en) * | 2003-12-06 | 2005-06-16 | Clariant Gmbh | Solvent based colorant preparations for ink jet printing |
| EP1593718A1 (en) * | 2004-05-06 | 2005-11-09 | Agfa-Gevaert | Radiation-curable ink-jet printing. |
| US20070152381A1 (en) * | 2003-12-23 | 2007-07-05 | Graziano Vignali | Process for colouring ceramic materials |
| KR20110045657A (en) * | 2009-10-27 | 2011-05-04 | 한국세라믹기술원 | Manufacturing method of nano ceramic pigment and manufacturing method of black matrix for plasma display panel |
| CN103333523A (en) * | 2013-06-08 | 2013-10-02 | 安徽天泰环保科技有限公司 | Method for preparing black iron oxide wrapped with silicon dioxide |
| CN104446654A (en) * | 2014-12-05 | 2015-03-25 | 武汉理工大学 | Method of preparing zirconium-based package type ceramic iron zircon pigment by virtue of organic network process |
| CN107474631A (en) * | 2017-09-19 | 2017-12-15 | 常州市卜诺赛机电技术有限公司 | A kind of ink-jet ceramic ink and preparation method thereof |
| CN107500740A (en) * | 2017-09-30 | 2017-12-22 | 佛山欧神诺陶瓷股份有限公司 | A kind of environment-friendly black Ceramic Tiles and preparation method thereof |
| CN108084796A (en) * | 2017-12-15 | 2018-05-29 | 佛山市扬子颜料有限公司 | A kind of new package carbon black ceramics marking ink and preparation method thereof |
| CN108456450A (en) * | 2018-03-01 | 2018-08-28 | 佛山市高明丰霖新型材料有限公司 | A kind of ceramic ink cobalt black colorant and preparation method thereof |
| CN108530992A (en) * | 2018-01-23 | 2018-09-14 | 佛山市华意陶瓷颜料有限公司 | A kind of black ceramic colorant, black ceramic ink and preparation method thereof |
| CN108912738A (en) * | 2018-06-06 | 2018-11-30 | 华南理工大学 | A kind of near-infrared high reflectance ceramic pigment and preparation method thereof |
| CN110655807A (en) * | 2019-09-29 | 2020-01-07 | 江西金环颜料有限公司 | Preparation method of zirconium silicate coated iron oxide red for ceramic ink-jet printing |
| CN111534152A (en) * | 2020-05-25 | 2020-08-14 | 佛山市三水区康立泰无机合成材料有限公司 | High-temperature-resistant black pigment for ceramic ink-jet printing, preparation method of high-temperature-resistant black pigment and ink for ceramic ink-jet printing |
| CN112063197A (en) * | 2020-08-18 | 2020-12-11 | 广东道氏技术股份有限公司 | Preparation method of zirconium silicate coated pigment for high-coating-rate ceramic ink-jet printing |
| CN113583513A (en) * | 2021-09-29 | 2021-11-02 | 佛山市三水区康立泰无机合成材料有限公司 | Black pigment for ceramic ink-jet printing and preparation method and application thereof |
| CN114921145A (en) * | 2022-06-10 | 2022-08-19 | 洛阳大豫实业有限公司 | Modified graphene anticorrosive paint and preparation method thereof |
| CN115572494A (en) * | 2022-09-27 | 2023-01-06 | 佛山市三水区康立泰无机合成材料有限公司 | Red-brown ceramic pigment, preparation method thereof and application of red-brown ceramic pigment in ceramic ink-jet printing ink |
-
2023
- 2023-04-04 CN CN202310352230.3A patent/CN116396636B/en active Active
Patent Citations (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005054381A1 (en) * | 2003-12-06 | 2005-06-16 | Clariant Gmbh | Solvent based colorant preparations for ink jet printing |
| US20070152381A1 (en) * | 2003-12-23 | 2007-07-05 | Graziano Vignali | Process for colouring ceramic materials |
| EP1593718A1 (en) * | 2004-05-06 | 2005-11-09 | Agfa-Gevaert | Radiation-curable ink-jet printing. |
| KR20110045657A (en) * | 2009-10-27 | 2011-05-04 | 한국세라믹기술원 | Manufacturing method of nano ceramic pigment and manufacturing method of black matrix for plasma display panel |
| CN103333523A (en) * | 2013-06-08 | 2013-10-02 | 安徽天泰环保科技有限公司 | Method for preparing black iron oxide wrapped with silicon dioxide |
| CN104446654A (en) * | 2014-12-05 | 2015-03-25 | 武汉理工大学 | Method of preparing zirconium-based package type ceramic iron zircon pigment by virtue of organic network process |
| CN107474631A (en) * | 2017-09-19 | 2017-12-15 | 常州市卜诺赛机电技术有限公司 | A kind of ink-jet ceramic ink and preparation method thereof |
| CN107500740A (en) * | 2017-09-30 | 2017-12-22 | 佛山欧神诺陶瓷股份有限公司 | A kind of environment-friendly black Ceramic Tiles and preparation method thereof |
| CN108084796A (en) * | 2017-12-15 | 2018-05-29 | 佛山市扬子颜料有限公司 | A kind of new package carbon black ceramics marking ink and preparation method thereof |
| CN108530992A (en) * | 2018-01-23 | 2018-09-14 | 佛山市华意陶瓷颜料有限公司 | A kind of black ceramic colorant, black ceramic ink and preparation method thereof |
| CN108456450A (en) * | 2018-03-01 | 2018-08-28 | 佛山市高明丰霖新型材料有限公司 | A kind of ceramic ink cobalt black colorant and preparation method thereof |
| CN108912738A (en) * | 2018-06-06 | 2018-11-30 | 华南理工大学 | A kind of near-infrared high reflectance ceramic pigment and preparation method thereof |
| CN110655807A (en) * | 2019-09-29 | 2020-01-07 | 江西金环颜料有限公司 | Preparation method of zirconium silicate coated iron oxide red for ceramic ink-jet printing |
| CN111534152A (en) * | 2020-05-25 | 2020-08-14 | 佛山市三水区康立泰无机合成材料有限公司 | High-temperature-resistant black pigment for ceramic ink-jet printing, preparation method of high-temperature-resistant black pigment and ink for ceramic ink-jet printing |
| CN112063197A (en) * | 2020-08-18 | 2020-12-11 | 广东道氏技术股份有限公司 | Preparation method of zirconium silicate coated pigment for high-coating-rate ceramic ink-jet printing |
| CN113583513A (en) * | 2021-09-29 | 2021-11-02 | 佛山市三水区康立泰无机合成材料有限公司 | Black pigment for ceramic ink-jet printing and preparation method and application thereof |
| CN114921145A (en) * | 2022-06-10 | 2022-08-19 | 洛阳大豫实业有限公司 | Modified graphene anticorrosive paint and preparation method thereof |
| CN115572494A (en) * | 2022-09-27 | 2023-01-06 | 佛山市三水区康立泰无机合成材料有限公司 | Red-brown ceramic pigment, preparation method thereof and application of red-brown ceramic pigment in ceramic ink-jet printing ink |
Non-Patent Citations (1)
| Title |
|---|
| 刘华锋;王慧;曾令可;: "黑色陶瓷色料的研究现状与展望", 中国陶瓷工业, no. 06, pages 39 - 41 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116396636B (en) | 2023-11-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108102427B (en) | Submicron cobalt-containing black ceramic pigment and preparation method and application thereof | |
| CN102199367B (en) | Method for preparing titanium dioxide pigment with high-temperature resistance | |
| CN106082671B (en) | Longquan celadon blueness glaze, Longquan celadon and preparation method thereof | |
| CN101139179B (en) | Ceramic coating burning colorful sand and method for making same | |
| CN105504883A (en) | Preparation method of high-temperature-resistant ferric oxide yellow pigment | |
| CN108084795A (en) | A kind of ceramic ink zaffre and preparation method thereof | |
| CN109054452A (en) | Copper-chromium black pigment and preparation method thereof | |
| CN110655807B (en) | Preparation method of zirconium silicate coated iron oxide red for ceramic ink-jet printing | |
| CN111875984B (en) | Preparation method of high-temperature-resistant iron oxide yellow pigment | |
| CN110951280A (en) | Copper-chromium black toner prepared by solid-phase sintering method promoted by molybdenum oxide and manganese oxide and preparation method thereof | |
| CN116396636B (en) | Black pigment for ceramic ink-jet printing and preparation method and application thereof | |
| CN108530992A (en) | A kind of black ceramic colorant, black ceramic ink and preparation method thereof | |
| CN110182818B (en) | Calcium-chromium garnet green pigment and preparation method thereof | |
| CN115572494B (en) | Red brown ceramic pigment, preparation method thereof and application thereof in ceramic inkjet printing ink | |
| CN110228823B (en) | Iron oxide yellow and preparation method thereof, and iron oxide red and preparation method thereof | |
| CN108456450B (en) | Cobalt black pigment for ceramic ink and preparation method thereof | |
| CN111534152A (en) | High-temperature-resistant black pigment for ceramic ink-jet printing, preparation method of high-temperature-resistant black pigment and ink for ceramic ink-jet printing | |
| CN111039324A (en) | Copper-chromium black and preparation method thereof | |
| CN109161227A (en) | A kind of preparation method of the reddish brown colorant of ceramic ink jet | |
| CN110204926A (en) | A kind of Vanadium zirconium blue ceramic pigment, Vanadium zirconium blue ceramic ink and preparation method thereof | |
| CN1137941C (en) | Preparing process of iron oxide red pigment for high-temperature ceramic with iron-containing industrial sludge | |
| CN111849207B (en) | Method for improving blue value of vanadium-zirconium blue pigment | |
| JP2003201122A (en) | Method for manufacturing granular hematite particle powder | |
| CN109021703B (en) | Bright red ceramic ink-jet pattern penetrating ink and preparation method thereof | |
| CN111285668A (en) | 3D printing ceramic slurry and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |