CN110437648A - A kind of width colour gamut is free of the blue ceramic pigment of chromium, cobalt, vanadium - Google Patents
A kind of width colour gamut is free of the blue ceramic pigment of chromium, cobalt, vanadium Download PDFInfo
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- CN110437648A CN110437648A CN201910851225.0A CN201910851225A CN110437648A CN 110437648 A CN110437648 A CN 110437648A CN 201910851225 A CN201910851225 A CN 201910851225A CN 110437648 A CN110437648 A CN 110437648A
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- cobalt
- chromium
- vanadium
- pigment
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0009—Pigments for ceramics
Abstract
The invention discloses the blue ceramic pigment that a kind of wide colour gamut is free of chromium, cobalt, vanadium, the Y of 22.4 ~ 49.3wt% is contained in the blue pigment2O3, the In of 8.9 ~ 35.7wt%2O3With the Mn of 1.7 ~ 21.3wt.%2O3, the present invention is with Y2O3、In2O3、Al2O3Yttrium-aluminium-garnet, yttrium indium aluminium composite garnet and the corundum of formation are as dispersible carrier, with Mn2O3For colorant, addition is in colour toners, mineralizer, fluxing agent, dispersing agent etc., suitably it is processed into a kind of new ceramics pigment, its performance indicator has biggish promotion than existing methods, b value reachable -40.4, can form more wide colour gamut, enrich color category, it is also safer without containing carcinogens, uses such as cobalts simultaneously.
Description
Technical field
The present invention relates to traditional ceramics decorative pigment fields more particularly to a kind of wide colour gamut to make pottery without the blue of chromium, cobalt, vanadium
Porcelain pigment.
Background technique
Pigment used in ceramic industry is a kind of special inorganic pigment, it necessarily be formed first certain specific structure or
Person is the ion coloring of certain stable states, secondly, it should the melt of resistance to glaze erosion, it is last it should under conditions of use with make
Matched with environment, such as uses temperature, thermal expansion coefficient etc..Therefore, the preparation of ceramic paint is complicated and stringent.
Blue is the pigment being commonly used in ceramic paint, and prior art blue pigment mainly has two major classes type, Yi Leishi
Vanadium zirconium blue pigment, color development characteristic are the inclined cyans of blue, and color saturation is low, such as color disclosed in patent CN109233339A
Material, chromaticity coordinate L is in 69.06 ~ 69.28, a in -11.72 ~ -12.37, b -23.95 ~ -25.01；Another kind of technology be with
Cobalt be color development element, though saturation degree with higher, lightness is lower, for example, cobalt blue ink disclosed in CN107033673A its
Color development coordinate is L:42.5 ~ 44, a:1.2 ~ 1.8, b:-26.5 ~ -29.8, the pigment color development gamut range of these two kinds of methods preparation
It is relatively narrow.In addition, in October, 2017, it is 2B class carcinogenic substance that world organization, which announces Cobalt and compounds of cobalt, for right in ceramic paint
There is security risk in producers and consumers.Therefore, it is necessary to develop a kind of new ceramic blue pigment, with wide color
Domain, while without containing toxic elements such as cobalts, to break through the limitation of existing colorant, ceramic decoration level is further increased, satisfaction disappears
The growing demand of the person of expense.
Summary of the invention
The purpose of the present invention is to overcome the deficiency in the prior art, provide a kind of wide colour gamut without chromium, cobalt, vanadium blue ceramic
Pigment, mainly with Y2O3、In2O3、Al2O3Yttrium-aluminium-garnet, yttrium indium aluminium composite garnet and the corundum of formation are carried as dispersion
Body, with Mn2O3For colorant, it is suitably processed into a kind of new ceramics pigment, performance indicator has larger than existing methods
Promotion, b value reachable -40.4, therefore can form more wide colour gamut enriches color category, while also causing without containing cobalt etc.
Cancer substance, use are safer.
The purpose of the present invention is achieved by the following technical programs:
A kind of wide colour gamut provided by the invention without chromium, cobalt, vanadium blue ceramic pigment, in the pigment containing 34.4 ~
The Y of 75.8wt%2O3, the In of 13.8 ~ 54.9wt%2O3With the Mn of 2.6 ~ 32.7wt.%2O3。
The present invention also provides a kind of more specifically wide colour gamut without chromium, cobalt, vanadium blue ceramic pigment, the pigment
Composition are as follows:
Dispersing agent of the present invention refers to common dispersing agent in ceramic pigment,.As the preferred embodiment of the invention, institute
It states dispersing agent and is selected from one or both of quartz or alpha-crystal form aluminium oxide.
As the preferred embodiment of the invention, the dispersing agent is quartz, and content is 12 ~ 67 wt.%.
As the preferred embodiment of the invention, the dispersing agent is alpha-crystal form aluminium oxide, and content is 7 ~ 35 wt.%.
The present invention also provides a kind of preparation methods of blue ceramic pigment, comprising the following steps:
(1) by Y2O3、In2O3And Mn2O3It is dry grinded in advance in merging ball mill to thin (10000-hole sieve tails over 0.05wt%)；
(2) ZnO(calcining is added in fine powder in step (1)), borax, dihydrogen phosphate, burn one of talcum or a variety of,
Then dispersing agent is added, the mixture of formation is dry grinded to thin (10000-hole sieve tails over 0.3wt%)；
(3) mixture prepared by step (2) is placed in refractory container and is heated to temperature T1, soaking time t1, wherein T1For
1050 ~ 1380 DEG C, t1For 30min ~ 12h；
(4) cooling take out of the calcined material of step (3) preparation is crushed；
(5) be added flux and water in the powder made from step (4), wet-milling is to all crossing 600 meshes, drying, pulverize to get.
Heating temperature T described in the preparation method of pigment of the present invention1, temperature value with pigment the different carry out phases of composition
The adjustment answered, with Mn2O3, ZnO(calcining), borax, dihydrogen phosphate, burn talcum mass ratio decline and correspondingly increase, and
Correspondingly increase with the rising of quartz and the mass ratio of alpha-crystal form aluminium oxide, grope by test of many times, temperature 1050 ~
1380 DEG C are suitable.
Soaking time t described in the preparation method of pigment of the present invention1, the time with pigment composition it is different carry out it is corresponding
Adjustment, with Mn2O3, ZnO(calcining), borax, dihydrogen phosphate, burn talcum mass ratio decline and accordingly extend, and with
Quartz and alpha-crystal form aluminium oxide mass ratio rising and accordingly extend, grope by test of many times, the time is in 30min ~ 12h.
Flux described in the preparation method of the bright pigment of the present invention, is flux common in ceramic pigment preparation process, is used
In color, powder enamel flux new in adjusting melting temperature, the performances, such as glaze such as coefficient of expansion, in-glaze decoration flux etc..Its dosage is ability
Well known to field technique personnel, in step (5), the mass ratio of powder, flux and water is preferably 7 ~ 20:30 ~ 43:50.
As the preferred embodiment of the invention, work as Mn2O3Content be higher than 4.7 wt.% when, what is be prepared is dark blue
Color, navy, black-and-blue pigment, need at this time by the multiple pickling of powder hydrochloric acid made from step (4) to supernatant liquor substantially without
Color, then it is washed to neutrality, it is dried for standby.The concentration of the hydrochloric acid is the common concentration of those skilled in the art, such as 6 ~ 18%.
Work as Mn2O3Content when being lower than 4.7 wt.%, what is prepared at this time is sapphirine, royalblue pigment, is not necessarily to pickling and washing.
The invention proposes a kind of innovations, without using chromium, cobalt, the new ceramics pigment of vanadium and its system in traditional technology
Preparation Method.Its advantages are specific as follows:
(1) present invention is with Y2O3、In2O3、Al2O3Yttrium-aluminium-garnet, yttrium indium aluminium composite garnet and the corundum of formation, which are used as, to be divided
Carrier is dissipated, by the Mn of itself and different proportion2O3, zinc oxide, burn talcum, the colorants such as quartz, in colour toners, mineralizer, fluxing
Agent, dispersing agent etc. are deployed, are calcined, available sapphirine, turquoise to partially red royalblue, navy, blue-black
A series of blue pigments such as color, b value reachable -40.4, color gamut is broad, and the color that can be formed is extremely abundant, and application range is more
Extensively.
(2) blue ceramic pigment prepared by the present invention, the more existing pigment of performance indicator have biggish promotion, product pellet
Dispersed high, colour generation is more preferable, while acid and alkali-resistance, corrosion-resistant, high temperature resistant, light shine, and preparation method is simple, and technique is controllable,
It is suitble to large-scale production, while raw materials used without containing carcinogenic or noxious materials such as cobalt, lead, chromium, it is environmentally protective.
Below in conjunction with embodiment, the present invention is described in further detail.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below.But this should not be interpreted as in the present invention
The range for stating theme is only limitted to embodiment below, all that model of the invention is belonged to based on the technology that the content of present invention is realized
It encloses.
Embodiment 1
Ceramic paint is prepared according to formula as below and preparation method.
(1) by Y2O3、In2O3And Mn2O3It is dry grinded in advance in merging ball mill to thin (10000-hole sieve tails over 0.05wt%)；
(2) alpha-crystal form aluminium oxide is added in fine powder in step (1), then adds dihydrogen phosphate and borax, formation mixes
Object is closed to dry grind to thin (10000-hole sieve tails over 0.3wt%)；
(3) mixture prepared by step (2) is placed in refractory container and is heated to 1380 DEG C of temperature, soaking time 12h；
(4) cooling take out of the calcined material of step (3) preparation is crushed；
(5) flux in-glaze decoration flux (common prescription are as follows: quartzy 12 boric acid 26 of feldspar 33 is added in the powder made from step (4)
24 barium carbonate of potassium nitrate, 18 strontium carbonate 17) and water, wherein the weight ratio of powder, flux and water is 20:30:50, wet-milling to whole
Cross 600 meshes, dry, pulverize to get.
Embodiment 2
Ceramic paint is prepared according to formula as below and preparation method.
(1) by Y2O3、In2O3And Mn2O3It is dry grinded in advance in merging ball mill to thin (10000-hole sieve tails over 0.05wt%)；
(2) borax and other raw materials are added in fine powder in step (1), the mixture of formation is dry grinded to carefully (10000-hole sieve tails over
0.3wt%)；
(3) mixture prepared by step (2) is placed in refractory container and is heated to 1050 DEG C, soaking time 30min；
(4) cooling take out of the calcined material of step (3) preparation is crushed, it is then multiple with 18% hydrochloric acid with 6% salt acid rinse diel
Pickling is substantially colorless to supernatant liquor, then is washed to neutrality, drying；
(5) overglaze color flux (common prescription are as follows: 60 boric acid of red lead, 20 quartz 12 aoxidizes is added in the powder made from step (4)
4 borax 4 of zinc) and water, wherein the weight ratio of powder, flux and water is 10:40:50, and wet-milling is dried to 600 meshes are all crossed,
Pulverize to get.
Embodiment 3
Ceramic paint is prepared according to formula as below and preparation method.
(1) by Y2O3、In2O3And Mn2O3It is dry grinded in advance in merging ball mill to thin (10000-hole sieve tails over 0.05wt%)；
(2) quartz and other raw materials are added in fine powder in step (1), the mixture of formation is dry grinded to carefully (10000-hole sieve tails over
0.3wt%)；
(3) mixture prepared by step (2) is placed in refractory container and is heated to 1200 DEG C of temperature, soaking time 2h；
(4) cooling take out of the calcined material of step (3) preparation is crushed；
(5) overglaze color flux (common prescription are as follows: 60 boric acid of red lead, 20 quartz 12 aoxidizes is added in the powder made from step (4)
4 borax 4 of zinc) and water, wherein the weight ratio of powder, flux and water is 10:40:50, and wet-milling is dried to 600 meshes are all crossed,
Pulverize to get.
Embodiment 4
Ceramic paint is prepared according to formula as below and preparation method.
(1) by Y2O3、In2O3And Mn2O3It is dry grinded in advance in merging ball mill to thin (10000-hole sieve tails over 0.05wt%)；
(2) alpha-crystal form aluminium oxide and other raw materials are added in fine powder in step (1), the mixture of formation is dry grinded to thin (ten thousand holes
Tail over 0.3wt%)；
(3) mixture prepared by step (2) is placed in refractory container and is heated to 1360 DEG C of temperature, soaking time 10h,
(4) cooling take out of the calcined material of step (3) preparation is crushed；
(5) flux in-glaze decoration flux (common prescription are as follows: quartzy 12 boric acid 26 of feldspar 33 is added in the powder made from step (4)
24 barium carbonate of potassium nitrate, 18 strontium carbonate 17) and water, wherein the weight ratio of powder, flux and water is 20:30:50, wet-milling to whole
Cross 600 meshes, dry, pulverize to get.
Embodiment 5
Ceramic paint is prepared according to formula as below and preparation method.
(1) by Y2O3、In2O3And Mn2O3It is dry grinded in advance in merging ball mill to thin (10000-hole sieve tails over 0.05wt%)；
(2) ZnO(calcining is added in fine powder in step (1)) other raw materials, the mixture of formation dry grinds to thin (10000-hole sieve sieve
Remaining 0.3wt%)；
(3) mixture prepared by step (2) is placed in refractory container and is heated to 1300 DEG C of temperature, soaking time 8.5h；
(4) cooling take out of the calcined material of step (3) preparation is crushed, it is then multiple with 18% hydrochloric acid with 6% salt acid rinse diel
Pickling is substantially colorless to supernatant liquor, then is washed to neutrality, drying；
(5) overglaze color flux (common prescription are as follows: 60 boric acid of red lead, 20 quartz 12 aoxidizes is added in the powder made from step (4)
4 borax 4 of zinc) and water, wherein the weight ratio of powder, flux and water is 10:40:50, and wet-milling is dried to 600 meshes are all crossed,
Pulverize to get.
Embodiment 6
Ceramic paint is prepared according to formula as below and preparation method.
(1) by Y2O3、In2O3And Mn2O3It is dry grinded in advance in merging ball mill to thin (10000-hole sieve tails over 0.05wt%)；
(2) dihydrogen phosphate is added in fine powder in step (1), burns talcum and alpha-crystal form aluminium oxide, the mixture dry grinding of formation
To thin (10000-hole sieve tails over 0.3wt%)；
(3) mixture prepared by step (2) is placed in refractory container and is heated to 1320 DEG C of temperature, soaking time 8.5h；
(4) cooling take out of the calcined material of step (3) preparation is crushed, it is then multiple with 18% hydrochloric acid with 6% salt acid rinse diel
Pickling is substantially colorless to supernatant liquor, then is washed to neutrality, drying；
(5) overglaze color flux (common prescription are as follows: 60 boric acid of red lead, 20 quartz 12 aoxidizes is added in the powder made from step (4)
4 borax 4 of zinc) and water, wherein the weight ratio of powder, flux and water is 10:40:50, and wet-milling is dried to 600 meshes are all crossed,
Pulverize to get.
Color development inspection, the blue pigment that will be made, on ceramic whiteware tire, by normal are carried out to the pigment of embodiment 1-6 preparation
Rule method colors in, and color in thickness 0.2-0.5mm, and decorating firing kiln 3~4.5h of color roasting is entered after dry, 800 DEG C of maximum temperature, cooling
Hair color effect is examined with color difference meter afterwards, the results are shown in Table 1.
1 embodiment colorant test result of table
The result shows that the Blue color domain that pigment prepared by the present invention is formed is broad, color includes brilliant blue, sapphire blue, acid blue, dark blue
The multicolour such as color, black-and-blue can mix a plurality of types of blue colors using method of the invention, can meet different face
The production of color needs, and production cost can be greatly reduced.
The pigment of embodiment preparation is tested for the property, 20h is impregnated using 5% hydrochloric acid solution and carries out acid resistance test；
120h, which is impregnated, using 5% sodium hydroxide solution carries out alkaline resistance properties test；Light shine examination is carried out using the ultraviolet light irradiation 120h of 600W
It tests；Thermal expansion coefficient is measured using German DIL402C thermodilatometric analysis instrument, the results are shown in Table 2.
The performance test results of 2 embodiment pigment of table
Experiments have shown that the blue ceramic pigment stable chemical performance of inventive formulation preparation, glossiness is good, lucuriant in design, and
Thermal expansion coefficient is lower, can be adapted with ceramic glaze, is the stable ceramic decoration material of a kind of new wide-gamut, performance, has
Extensive promotional value.
Claims (7)
1. a kind of width colour gamut without chromium, cobalt, vanadium blue ceramic pigment, it is characterised in that in the blue containing 22.4 ~
The Y of 49.3wt%2O3, the In of 8.9 ~ 35.7wt%2O3With the Mn of 1.7 ~ 21.3wt.%2O3。
2. the blue ceramic pigment that width colour gamut according to claim 1 is free of chromium, cobalt, vanadium, it is characterised in that the pigment
Composition are as follows:
。
3. the blue ceramic pigment that width colour gamut according to claim 2 is free of chromium, cobalt, vanadium, it is characterised in that the dispersion
Agent is selected from one or both of quartz or alpha-crystal form aluminium oxide.
4. the blue ceramic pigment that width colour gamut according to claim 3 is free of chromium, cobalt, vanadium, it is characterised in that the dispersion
Agent is quartz, and content is 12 ~ 67 wt.%.
5. the blue ceramic pigment that width colour gamut according to claim 3 is free of chromium, cobalt, vanadium, it is characterised in that the dispersion
Agent is alpha-crystal form aluminium oxide, and content is 7 ~ 35 wt.%.
6. the blue ceramic pigment that width colour gamut according to claim 3 is free of chromium, cobalt, vanadium, it is characterised in that the pigment
Preparation method the following steps are included:
(1) by Y2O3、In2O3And Mn2O3It is dry grinded in advance in merging ball mill to thin (10000-hole sieve tails over 0.05wt%)；
(2) ZnO(calcining is added in fine powder in step (1)), borax, dihydrogen phosphate, burn one of talcum or a variety of,
Then dispersing agent is added, the mixture of formation is dry grinded to thin (10000-hole sieve tails over 0.3wt%)；
(3) mixture prepared by step (2) is placed in refractory container and is heated to temperature T1, soaking time t1, wherein T1For
1050 ~ 1380 DEG C, t1For 30min ~ 12h；
(4) cooling take out of the calcined material of step (3) preparation is crushed；
(5) be added flux and water in the powder made from step (4), wet-milling is to all crossing 600 meshes, drying, pulverize to get.
7. width colour gamut according to claim 6 without chromium, cobalt, vanadium blue ceramic pigment preparation method, feature exists
In working as Mn2O3Content be higher than 4.7 wt.% when, need to be by the multiple pickling of powder hydrochloric acid made from step (4) to supernatant liquor base
This is colourless, then is washed to neutrality, is dried for standby.
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| CN201910851225.0A CN110437648A (en) | 2019-09-10 | 2019-09-10 | A kind of width colour gamut is free of the blue ceramic pigment of chromium, cobalt, vanadium |
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| CN201910851225.0A CN110437648A (en) | 2019-09-10 | 2019-09-10 | A kind of width colour gamut is free of the blue ceramic pigment of chromium, cobalt, vanadium |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110922788A (en) * | 2019-12-09 | 2020-03-27 | 中国科学院包头稀土研发中心 | Inorganic oxide dark green colorant and preparation method and application thereof |
| CN111040470A (en) * | 2019-12-17 | 2020-04-21 | 佛山科学技术学院 | Blue inorganic pigment and preparation method thereof |
| CN111170763A (en) * | 2020-01-19 | 2020-05-19 | 湖南东豪先进陶瓷材料有限公司 | Ceramic glaze color fixative and preparation method thereof |
| CN111849204A (en) * | 2020-07-28 | 2020-10-30 | 淄博科睿特新材料科技有限公司 | Chromophoric group cobalt-free blue glass pigment and method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110922788A (en) * | 2019-12-09 | 2020-03-27 | 中国科学院包头稀土研发中心 | Inorganic oxide dark green colorant and preparation method and application thereof |
| CN110922788B (en) * | 2019-12-09 | 2021-04-20 | 中国科学院包头稀土研发中心 | Inorganic oxide dark green colorant and preparation method and application thereof |
| CN111040470A (en) * | 2019-12-17 | 2020-04-21 | 佛山科学技术学院 | Blue inorganic pigment and preparation method thereof |
| CN111040470B (en) * | 2019-12-17 | 2021-03-26 | 佛山科学技术学院 | Blue inorganic pigment and preparation method thereof |
| CN111170763A (en) * | 2020-01-19 | 2020-05-19 | 湖南东豪先进陶瓷材料有限公司 | Ceramic glaze color fixative and preparation method thereof |
| CN111849204A (en) * | 2020-07-28 | 2020-10-30 | 淄博科睿特新材料科技有限公司 | Chromophoric group cobalt-free blue glass pigment and method |
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Application publication date: 20191112 |