CN108929033A - A kind of glass-ceramic colorant and preparation method thereof with discoloration effect - Google Patents
A kind of glass-ceramic colorant and preparation method thereof with discoloration effect Download PDFInfo
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- CN108929033A CN108929033A CN201810784075.1A CN201810784075A CN108929033A CN 108929033 A CN108929033 A CN 108929033A CN 201810784075 A CN201810784075 A CN 201810784075A CN 108929033 A CN108929033 A CN 108929033A
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- glass
- preparation
- discoloration effect
- ceramic colorant
- colorant
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/04—Opacifiers, e.g. fluorides or phosphates; Pigments
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7756—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing neodynium
- C09K11/7757—Halogenides
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
Abstract
The invention discloses a kind of glass-ceramic colorant and preparation method thereof with discoloration effect.The preparation method of the glass-ceramic colorant with discoloration effect includes the following steps: that (1) accurately weighs molybdenum compound raw material and neodymia raw material according to the ratio, and mineralizer and grinding distribution liquid is added, using high-energy density Ball-stirring mill wet grinding, mill base slurry is obtained;(2) gained mill base slurry is placed in air dry oven to be dried, obtains dried material;(3) dried material is subjected to high-temperature calcination, obtains calcining materials;(4) calcining materials are crushed, wash and be drying to obtain the glass-ceramic colorant with discoloration effect.Preparation method raw material of the invention is easy to get, and simple process is conducive to industrial applications.And the glass-ceramic colorant color development with discoloration effect prepared according to the method described above is stablized, color changeable effect is good.
Description
Technical field
The invention belongs to ceramics, glass enamel material technical field more particularly to a kind of glass-ceramics with discoloration effect
Colorant and preparation method thereof.
Background technique
Inkjet printing technology is a kind of contactless digital printing technologies succeeded in developing late 1970s.It will
Ink is ejected on various dielectric surfaces by the nozzle on print head, realize non-contact, high speed, the monochrome of low noise and
Colored writings and image printing.Opposite Conventional printing process, has abandoned the cumbersome of Conventional decal mode, has improved the essence of stamp
Degree, and image appearance is finer and smoother true, no version is efficient, is more suitable current building decoration materials fashion, personalization, art
Change, small lot, multi-color, high emulation, the developing trend of low-carbon environment-friendly.The successful application of digital ink-jet printed technology is building dress
Exterior material manufactures a new milestone of processing technology, and construction material decoration technique is pushed to a brand-new stage.
Since China in 2009 introduces First ceramic ink jet machine, the development of ceramic ink jet printing technology is advanced by leaps and bounds,
It has been widely used now.Meanwhile the glass printing ink of the research and development of offshore company in 2012 is directly outdoors or indoor
Digital printing technologies are carried out on decoration glass and are introduced into China, indicate inkjet printing technology formally in China glass decoration field
It is applied.By the development of many years, the pattern decorative effect of construction material is far from meeting people to inkjet printing skill
The expectation of art application, more emphasis artistic effect and special decorative effect.
Glass-ceramic colorant with discoloration effect can be applied to inkjet printing technology field, so that ceramic/glass material
The decorative pattern that different visual perceptions can be showed after material decoration under different light sources greatly improves ceramic/glass decoration
The artistic effect of material.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of glass-ceramic colorant with discoloration effect
Preparation method.
It is another object of the present invention to provide the glass-ceramic colors with discoloration effect that above-mentioned preparation method obtains
Material.
The purpose of the present invention adopts the following technical solutions to achieve.
A kind of preparation method of the glass-ceramic colorant with discoloration effect, includes the following steps:
1) molybdenum compound and neodymia raw material are accurately weighed according to the ratio, and mineralizer and grinding distribution liquid is added, using high-energy
Density Ball-stirring mill wet grinding, obtains mill base slurry;
2) gained mill base slurry is placed in air dry oven to be dried, obtains dried material;
3) dried material is subjected to high-temperature calcination, obtains calcining materials;
4) calcining materials are crushed, wash and be drying to obtain the glass-ceramic colorant with discoloration effect;
Preferably, the molar ratio of molybdenum compound described in step (1) and neodymia raw material molybdenum neodymium element are as follows: molybdenum: neodymium=1:(2~
3).
Preferably, mineralizer described in step (1) is one in sodium fluoride, potassium fluoride, calcirm-fluoride, lithium fluoride and magnesium fluoride
Kind and any combination thereof.
Preferably, the additive amount of mineralizer described in step (1) is the 0.5%~10% of the raw material butt quality.
Preferably, grinding distribution liquid is the mixing liquid of dispersing agent and water in step (1), and dispersing agent is aqueous organic dispersion
Agent, dispersant are the 3%~10% of the raw material butt quality.
Preferably, milling time described in step (1) is 1~4 hour.
Preferably, drying temperature described in step (2) is 100 DEG C, and drying time is 10~24 hours.
Preferably, high-temperature calcination temperature described in step (3) is 1000~1400 DEG C, and calcination time is 1~6 hour.
Preferably, the solvent of step (4) washing process is dilute nitric acid solution and water.
Compared with prior art, the beneficial effects of the present invention are:
(1) molybdenum compound and neodymia easily form the crystalline structure of diversified forms at high temperature, and different crystalline structure color developments has
Notable difference.Preparation method of the present invention can be obtained by introducing mineralizer within the scope of wider raw material proportioning
Fully reacting and the single colorant of crystalline structure, it is ensured that color development is stablized, while can reduce the synthesis temperature of colorant.
(2) preparation method of the present invention handles raw material using high-energy density Ball-stirring mill, can make raw material average grain diameter
Less than 500 nanometers, increase the contact area and uniformity coefficient of reaction raw materials, the subsequent synthesis temperature for advantageously reducing colorant is timely
Between, and guarantee the uniformity of colorant granularity.
(3) dispersing agent of grinding distribution liquid is aqueous organic dispersing agent in preparation method of the present invention, and dispersion efficiency is high,
And impurity component will not be introduced to reaction system.
(4) preparation method raw material of the present invention is easy to get, and simple process, production cost is low, the glass-ceramic colorant of preparation
Color development is stablized, and industrialized production and application are conducive to.
Specific embodiment
Below with reference to embodiment, implementation of the invention is further described, but embodiments of the present invention are not limited to
This.
Embodiment 1
A kind of glass-ceramic colorant with discoloration effect, preparation method are as follows:
(1) 14.4g molybdenum trioxide and 33.6g neodymia are weighed, 0.48g sodium fluoride and 100g grinding distribution liquid (dispersing agent is added
For Tego757W, content is the 3% of raw material butt quality), using high-energy density Ball-stirring mill wet grinding 2 hours, ground
Slurry (average grain diameter is 468.7 nanometers);
(2) gained grinding slurry is placed in drying 14 hours in 100 DEG C of air dry ovens, is dried to moisture content and is lower than
0.5wt% obtains dried material;
(3) dried material is crushed, and in 1350 DEG C of temperature lower calcination 5 hours, obtains calcining materials after cooling;
(4) calcining materials are crushed, and successively uses dilute nitric acid solution and water washing, the pottery with discoloration effect is obtained after dry
Porcelain glass pigment.
There is the glass-ceramic colorant epigranular of discoloration effect, color development is stablized, and is under fluorescent light obtained by the present embodiment
Leaf green is in olive-gray under sunlight, is in lotus root starch color under incandescence light, is in yellow green at shop light source (TL84).
The Lab value that gained colorant under different light sources is tested with color difference meter, in addition under two kinds of light sources of fluorescent lamp and shop light source (TL84)
Except value of chromatism Δ E < 5, for the value of chromatism Δ E under light source between 8 to 20, the color changeable effect under different light sources is bright two-by-two for other
It is aobvious.Meanwhile gained colorant is through overpickling and high-temperature calcination, chemical stability and good heat stability.
Embodiment 2
A kind of glass-ceramic colorant with discoloration effect, preparation method are as follows:
(1) 12.4g ammonium heptamolybdate and 29.4g neodymia are weighed, 2.5g potassium fluoride and 100g grinding distribution liquid is added, and (dispersing agent is
BYK2010, content are the 10% of raw material butt quality), using high-energy density Ball-stirring mill wet grinding 4 hours, obtain slurry
Material (average grain diameter is 231.2 nanometers);
(2) gained grinding slurry is placed in drying 18 hours in 100 DEG C of air dry ovens, is dried to moisture content lower than 0.5
Wt% obtains dried material;
(3) dried material is crushed, and in 1000 DEG C of temperature lower calcination 3 hours, obtains calcining materials after cooling;
(4) calcining materials are crushed, and successively uses dust technology and water washing, the ceramic glass with discoloration effect is obtained after dry
Glass colorant.
There is the glass-ceramic colorant epigranular of discoloration effect, color development is stablized, and is under fluorescent light obtained by the present embodiment
Leaf green is in olive-gray under sunlight, is in lotus root starch color under incandescence light, is in yellow green at shop light source (TL84).
The Lab value that gained colorant under different light sources is tested with color difference meter, in addition under two kinds of light sources of fluorescent lamp and shop light source (TL84)
Except value of chromatism Δ E < 5, for the value of chromatism Δ E under light source between 8 to 20, the color changeable effect under different light sources is bright two-by-two for other
It is aobvious.Meanwhile gained colorant is through overpickling and high-temperature calcination, chemical stability and good heat stability.
Embodiment 3
A kind of glass-ceramic colorant with discoloration effect, preparation method are as follows:
(1) 13.3g ammonium tetramolybdate and 40.4g neodymia are weighed, 2.7g lithium fluoride is added and 100g grinding distribution liquid (wherein disperses
Agent is AFCONA4595, and content is the 5% of raw material butt quality), using high-energy density Ball-stirring mill wet grinding 3 hours, obtain
Grinding slurry (average grain diameter is 390.6 nanometers);
(2) gained grinding slurry is placed in drying 10 hours in 100 DEG C of air dry ovens, is dried to moisture content lower than 0.5
Wt% obtains dried material;
(3) dried material is crushed, and in 1100 DEG C of temperature lower calcination 5 hours, obtains calcining materials after cooling;
(4) calcining materials are crushed, and successively uses dust technology and water washing, the ceramic glass with discoloration effect is obtained after dry
Glass colorant.
There is the glass-ceramic colorant epigranular of discoloration effect, color development is stablized, and is under fluorescent light obtained by the present embodiment
Leaf green is in olive-gray under sunlight, is in lotus root starch color under incandescence light, is in yellow green at shop light source (TL84).
The Lab value that gained colorant under different light sources is tested with color difference meter, in addition under two kinds of light sources of fluorescent lamp and shop light source (TL84)
Except value of chromatism Δ E < 5, for the value of chromatism Δ E under light source between 8 to 20, the color changeable effect under different light sources is bright two-by-two for other
It is aobvious.Meanwhile gained colorant is through overpickling and high-temperature calcination, chemical stability and good heat stability.
Embodiment 4
A kind of glass-ceramic colorant with discoloration effect, preparation method are as follows:
(1) 14.4g molybdenum trioxide and 36.6g neodymia are weighed, 3.8g calcirm-fluoride is added and 100g grinding distribution liquid (wherein disperses
Agent is TEGO 755W, and content is the 8% of raw material butt quality), using high-energy density Ball-stirring mill wet grinding 3 hours, obtain
Grinding slurry (average grain diameter is 315.3 nanometers);
(2) gained grinding slurry is placed in drying 12 hours in 100 DEG C of air dry ovens, is dried to moisture content lower than 0.5
Wt% obtains dried material;
(3) dried material is crushed, and in 1200 DEG C of temperature lower calcination 5 hours, obtains calcining materials after cooling;
(4) calcining materials are crushed, and successively uses dust technology and water washing, the ceramic glass with discoloration effect is obtained after dry
Glass colorant.
There is the glass-ceramic colorant epigranular of discoloration effect, color development is stablized, and is under fluorescent light obtained by the present embodiment
Leaf green is in olive-gray under sunlight, is in lotus root starch color under incandescence light, is in yellow green at shop light source (TL84).
The Lab value that gained colorant under different light sources is tested with color difference meter, in addition under two kinds of light sources of fluorescent lamp and shop light source (TL84)
Except value of chromatism Δ E < 5, for the value of chromatism Δ E under light source between 8 to 20, the color changeable effect under different light sources is bright two-by-two for other
It is aobvious.Meanwhile gained colorant is through overpickling and high-temperature calcination, chemical stability and good heat stability.
Comparative example 1
A kind of glass-ceramic colorant with discoloration effect, preparation method are as follows:
(1) 14.4g molybdenum trioxide and 33.6g neodymia are weighed, 0.48g sodium fluoride and 50g grinding distribution liquid is added, and (dispersing agent is
TEGO757W, content are the 3% of raw material butt quality), 30min is ground using agate, material is sufficiently mixed uniformly, is ground
Defibrination material (average grain diameter is 12.3 microns);
(2) gained grinding slurry is placed in drying 14 hours in 100 DEG C of air dry ovens, is dried to moisture content lower than 0.5
Wt% obtains dried material;
(3) dried material is crushed, and in 1350 DEG C of temperature lower calcination 5 hours, obtains calcining materials after cooling;
(4) calcining materials are crushed, and successively uses dilute nitric acid solution and water washing, it is dry.
Glass-ceramic colorant granularity obtained by the present embodiment is uneven, and not exclusively, product is the mixing of the colors such as green purple for reaction
Object.
Comparative example 2
A kind of glass-ceramic colorant with discoloration effect, preparation method are as follows:
(1) 12.4g ammonium heptamolybdate and 29.4g neodymia are weighed, adding 100g grinding distribution liquid, (dispersing agent BYK2010, content are
The 10% of raw material butt quality), using high-energy density Ball-stirring mill wet grinding 4 hours, obtaining grinding slurry, (average grain diameter was
227.9 nanometers);
(2) gained grinding slurry is placed in drying 18 hours in 100 DEG C of air dry ovens, is dried to moisture content lower than 0.5
Wt% obtains dried material;
(3) dried material is crushed, and in 1000 DEG C of temperature lower calcination 3 hours, obtains calcining materials after cooling;
(4) calcining materials are crushed, and successively uses dust technology and water washing, it is dry.
Glass-ceramic colorant granularity obtained by the present embodiment is uneven, and not exclusively, product is the mixing of the colors such as green purple for reaction
Object.
Claims (10)
1. a kind of preparation method of the glass-ceramic colorant with discoloration effect, which comprises the steps of:
(1) molybdenum compound raw material and neodymia raw material are weighed, and mineralizer and grinding distribution liquid is added, is stirred using high-energy density
Mill wet grinding is mixed, mill base slurry is obtained;
(2) gained mill base slurry is dry, obtain dried material;
(3) dried material is subjected to high-temperature calcination, obtains calcining materials;
(4) calcining materials are crushed, washs and dry to get the glass-ceramic colorant with discoloration effect.
2. a kind of preparation method of glass-ceramic colorant with discoloration effect according to claim 1, it is characterised in that:
The molar ratio of molybdenum neodymium element is molybdenum: neodymium=1:(2~3 in molybdenum compound described in step (1) and neodymia raw material).
3. a kind of preparation method of glass-ceramic colorant with discoloration effect according to claim 1, it is characterised in that:
Molybdenum compound raw material described in step (1) is in ammonium dimolybdate, ammonium tetramolybdate, ammonium heptamolybdate, ammonium octamolybdate and molybdenum trioxide
It is one or more.
4. a kind of preparation method of glass-ceramic colorant with discoloration effect according to claim 1, it is characterised in that:
Mineralizer described in step (1) is one of sodium fluoride, potassium fluoride, calcirm-fluoride, lithium fluoride and magnesium fluoride or a variety of.
5. a kind of preparation method of glass-ceramic colorant with discoloration effect according to claim 1, it is characterised in that:
The additive amount of mineralizer described in step (1) is the 0.5%~10% of the raw material butt quality.
6. a kind of preparation method of glass-ceramic colorant with discoloration effect according to claim 1, it is characterised in that:
Grinding distribution liquid is the mixing liquid of aqueous organic dispersing agent and water in step (1), wherein aqueous organic dispersing agent is the original
Expect the 3%~10% of butt quality.
7. a kind of preparation method of glass-ceramic colorant with discoloration effect according to claim 1, it is characterised in that:
The time of step (1) described grinding is 1~4 hour.
8. a kind of preparation method of glass-ceramic colorant with discoloration effect according to claim 1, it is characterised in that:
The temperature of step (2) described drying is 100 DEG C, and the dry time is 10~24 hours.
9. a kind of preparation method of glass-ceramic colorant with discoloration effect according to claim 1, it is characterised in that:
The temperature of step (3) described high-temperature calcination is 1000~1400 DEG C, and calcination time is 1~6 hour.
10. a kind of glass-ceramic color with discoloration effect as made from preparation method according to any one of claims 1 to 9
Material.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112850790A (en) * | 2021-02-01 | 2021-05-28 | 成都虹波钼业有限责任公司 | Molybdenum trioxide for high-solubility catalyst and production process thereof |
CN112940536A (en) * | 2021-03-11 | 2021-06-11 | 华南理工大学 | Inorganic functional pigment with high near-infrared reflectivity and color change effect and preparation and application thereof |
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CN104311147A (en) * | 2014-10-14 | 2015-01-28 | 华南理工大学 | High-temperature ceramic pigment having color change effect and preparation method of ceramic pigment |
CN106189517A (en) * | 2016-08-29 | 2016-12-07 | 佛山市高明区海帝陶瓷原料有限公司 | A kind of photochromic ceramic ink with leather pattern effect and preparation method thereof |
US10661550B2 (en) * | 2014-06-27 | 2020-05-26 | Fujimi Incorporated | Molding material for forming structure and molding method |
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2018
- 2018-07-17 CN CN201810784075.1A patent/CN108929033A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2008021495A2 (en) * | 2006-08-18 | 2008-02-21 | Pentron Ceramics, Inc. | Coloring of ceramics by atmosphere control |
US10661550B2 (en) * | 2014-06-27 | 2020-05-26 | Fujimi Incorporated | Molding material for forming structure and molding method |
CN104311147A (en) * | 2014-10-14 | 2015-01-28 | 华南理工大学 | High-temperature ceramic pigment having color change effect and preparation method of ceramic pigment |
CN106189517A (en) * | 2016-08-29 | 2016-12-07 | 佛山市高明区海帝陶瓷原料有限公司 | A kind of photochromic ceramic ink with leather pattern effect and preparation method thereof |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112850790A (en) * | 2021-02-01 | 2021-05-28 | 成都虹波钼业有限责任公司 | Molybdenum trioxide for high-solubility catalyst and production process thereof |
CN112940536A (en) * | 2021-03-11 | 2021-06-11 | 华南理工大学 | Inorganic functional pigment with high near-infrared reflectivity and color change effect and preparation and application thereof |
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