CN107936618A - A kind of fused salt auxiliary prepares the method for zirconium silicate parcel carbon black colorant and its obtained product - Google Patents
A kind of fused salt auxiliary prepares the method for zirconium silicate parcel carbon black colorant and its obtained product Download PDFInfo
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- CN107936618A CN107936618A CN201711197887.8A CN201711197887A CN107936618A CN 107936618 A CN107936618 A CN 107936618A CN 201711197887 A CN201711197887 A CN 201711197887A CN 107936618 A CN107936618 A CN 107936618A
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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
- C09C1/0012—Pigments for ceramics containing zirconium and silicon
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Abstract
The invention discloses a kind of method that fused salt auxiliary prepares zirconium silicate parcel carbon black colorant, zirconium silicate colloidal sol is prepared by sol-gal process, then add carbon source and fused salt is uniformly mixed, the mixture that zirconium silicate gel uniformly coats carbon black or carbon black presoma is obtained after dry；After obtained through high-temperature heat treatment zirconium silicate parcel carbon black colorant.In addition, also disclosing product made from the method for zirconium silicate parcel carbon black colorant is prepared using above-mentioned fused salt auxiliary.The present invention has the advantages of technique is simple, and raw material is inexpensive, derives from a wealth of sources；The colorant product encapsulation ratio height and compact structure, pure color obtained, may be directly applied to the coloring in ceramic glaze or in base, so as to be effectively facilitated the application of ceramic pigment and development.
Description
Technical field
The present invention relates to ceramic pigment technical field, more particularly to a kind of preparation method of zirconium silicate parcel carbon black colorant and
Its obtained product.
Background technology
Ceramic pigment refers to the coloured special color material of ceramics of powdery being formulated with color base and flux or additive, can
To be directly used in ceramic body and glaze layer coloring.At present, black ceramic colorant accounts for the 25% of the ceramic pigment market share, with biography
System spinel-type black pigment is compared, and coated black ceramic colorant is caused without variable valency metal elements such as cobalt and chromium
The extensive concern of people.This kind of coated black ceramic colorant of the prior art, generally use carbon black powder have as colouring agent
Good color development ability, and zirconium silicate (or silica) crystal as shell can be aoxidized at high temperature to avoid carbon black.Cause
This, the finely regulating for core shell structure is the committed step for preparing black occlusion pigment.At present, the prior art prepares zirconium silicate
The method for wrapping up carbon black colorant is mainly liquid phase method, i.e., carbon black powder or predecessor is dispersed in zirconium silicate colloidal sol, through overdrying
Occlusion pigment is obtained after dry, high temperature non-oxygenated atmosphere calcining.But there are still following deficiency for these methods：First, silicon under high temperature
Sour zirconium crystal growth is difficult to control, and mass transfer is more difficult；Second, carbon black and silicon fluoride (silica and mineralizer lithium fluoride generate) easy oxygen
Change and volatilization, cause colour former to reduce and the problems such as package structure is not fine and close, thus cause the colorant encapsulation ratio prepared it is relatively low,
Colourity is poor.
Fused salt refers to the molten mass formed after salt fusing, is usually made of metal cation and metalloid anion.
Fused salt, which is heated, can be melt into liquid, be conducive to the anisotropic growth of crystal, thus is commonly used to synthesis nanometer rods, whisker, receives
The monodimension nanometer materials such as rice band.At present, it there is no the report that zirconium silicate parcel carbon black colorant is prepared using molten-salt growth method.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of fused salt auxiliary to prepare zirconium silicate parcel carbon black
The method of colorant, the liquid phase environment for being conducive to zirconium silicate mass transfer is created by fused salt high temperature melting, while avoids silicon fluoride and charcoal
Black volatilization, so as to obtain encapsulation ratio height, the coated carbon black colorant of pure color.Another object of the present invention is to provide profit
The product made from above-mentioned fused salt auxiliary prepares the method for zirconium silicate parcel carbon black colorant.
The purpose of the present invention is achieved by the following technical programs：
The method that a kind of fused salt auxiliary provided by the invention prepares zirconium silicate parcel carbon black colorant, comprises the following steps：
(1) silicon source and zirconium source are dissolved in water or organic solvent according to stoichiometric ratio formed molar concentration for 0.05~
The silicic acid zirconium solution of 3.0mol/L, and mineralizer is added, after being uniformly mixed zirconium silicate colloidal sol is obtained through sol-gel process；
(2) carbon source and fused salt are added in the zirconium silicate colloidal sol, according to zirconium silicate described in mass ratio: carbon source: fused salt=1
: 0.01~1: 1~6, solution is evaporated at a temperature of 80~150 DEG C after mixing, before obtaining zirconium silicate parcel carbon black
Drive thing；
(3) zirconium silicate parcel carbon black predecessor is heat-treated under nonoxidizing atmosphere, furnace cooling, is mixed
Close powder；
(4) mixed powder is through pickling, washing, and after being heat-treated under oxidizing atmosphere, furnace cooling, that is, obtain silicon
Sour zirconium wraps up carbon black colorant.
The present invention prepares zirconium silicate parcel carbon black colorant using fused salt auxiliary, prepares silicon by sol-gel process first
Sour zirconium colloidal sol, then adds carbon source and fused salt is uniformly mixed, so that zirconium silicate colloidal sol is uniformly wrapped on carbon black or carbon black after dry
Presoma surface；Meanwhile in the liquid phase environment that fused salt high temperature melting is created, zirconium silicate crystal is in carbon black or carbon black presoma
Surface Crystallization；And as high-temperature molten salt volatilization causes degree of supersaturation to increase so that zirconium silicate crystal is constantly grown around core,
So as to be conducive to obtain the zirconium silicate parcel carbon black colorant of core shell structure.
Further, in step (1) of the present invention, the organic solvent is ethanol, normal propyl alcohol or acetic acid；It is described molten
Glue-gel process is directly heats or solvent thermal reaction, and temperature is 70~100 DEG C, and the reaction time is 1~24h.The mineralizer
Dosage be zirconium silicate 1.5~7.0wt%.
Further, silicon source of the present invention is ethyl orthosilicate, silicon tetrachloride, waterglass, silane coupling agent or inclined silicon
Sour sodium；The zirconium source is zirconium chloride, zirconium oxychloride, acetic acid zirconium, zirconium sulfate, zirconium nitrate, zirconium-n-propylate or zirconium iso-propoxide.It is described
Mineralizer is lithium fluoride, magnesium fluoride, sodium fluoride, calcirm-fluoride or lithium chloride.
Further, carbon source of the present invention for carbon black powder, phenolic resin, plant fiber, sucrose, fructose, glucose,
Or starch.The fused salt is that alkali tungstates, alkali metal molybdate, one kind in alkali metal chloride or its combination are formed
Composite fused salt；The alkali metal is respectively lithium, sodium, potassium element.When forming composite fused salt using two kinds of fused salts, according to quality than it
Ratio is 1~9: 1~9.
In such scheme, in step (3) of the present invention, heat treating regime is 3~5 DEG C/min under the nonoxidizing atmosphere
It is warming up to 800~1050 DEG C of 1~4h of insulation；In the step (4), heat treating regime is 3~5 DEG C/min under the oxidizing atmosphere
It is warming up to 700~900 DEG C of 1~4h of insulation.
Another object of the present invention is achieved by the following technical programs：
Product made from the method for zirconium silicate parcel carbon black colorant, the colorant product shape are prepared using above-mentioned fused salt auxiliary
Looks size uniform is tiny, and particle diameter is 0.5~5 μm.
The invention has the advantages that：
(1) present invention prepares zirconium silicate parcel carbon black colorant using fused salt auxiliary, is created by fused salt high temperature melting
Liquid phase environment, is conducive to zirconium silicate mass transfer, while is also beneficial to carbon black or carbon precursor, silicon fluoride and oxygen-barrier, avoids
The volatilization of silicon fluoride and carbon black, so as to add the carbon left of colorant, obtains the excellent black occlusion pigment of colour generation.
(2) with the volatilization of fused salt, degree of supersaturation increase, the isotropic growth journey of zirconium silicate crystal under high temperature of the present invention
Degree enhancing, zirconium silicate crystal are constantly grown around core, the occlusion pigment of core shell structure are advantageously formed, so as to efficiently solve
The problem of prior art encapsulation ratio is low.Product encapsulation ratio height of the present invention and compact structure, pure color (L*Reach 28.34~
36.01) coloring in ceramic glaze or in base, is may be directly applied to, so as to effectively facilitate the application of ceramic pigment
And development.
(3) present invention has the advantages of technique is simple, and raw material is inexpensive, derives from a wealth of sources, and has broad application prospects.
Brief description of the drawings
Below in conjunction with embodiment and attached drawing, the present invention is described in further detail：
Fig. 1 is the XRD spectrum of zirconium silicate parcel carbon black colorant prepared by the embodiment of the present invention one；
Fig. 2 is the SEM photograph of zirconium silicate parcel carbon black colorant prepared by the embodiment of the present invention one；
Fig. 3 is the CIEL of zirconium silicate parcel carbon black colorant prepared by the embodiment of the present invention one*a*b*Curve map；
Fig. 4 is the XRD spectrum of zirconium silicate parcel carbon black colorant prepared by the embodiment of the present invention two；
Fig. 5 is the SEM photograph of zirconium silicate parcel carbon black colorant prepared by the embodiment of the present invention two；
Fig. 6 is the XRD spectrum of zirconium silicate parcel carbon black colorant prepared by the embodiment of the present invention three；
Fig. 7 is the XRD spectrum of zirconium silicate parcel carbon black colorant prepared by the embodiment of the present invention four.
Embodiment
Embodiment one：
The method that a kind of fused salt auxiliary of the present embodiment prepares zirconium silicate parcel carbon black colorant, its step are as follows：
(1) 10.56g zirconium chlorides and 10mL ethyl orthosilicates are dissolved in 45mL ethanol, it is 1.0mol/L to form concentration
Silicic acid zirconium solution, then add 0.43g lithium fluoride (for the 5.21wt% of zirconium silicate), after mixing at a temperature of 100 DEG C
It is heated at reflux 8h and obtains zirconium silicate colloidal sol；
(2) weigh 1.65g, 3.30g, 4.95g, 6.60g, 8.25g phenolic resin (be respectively zirconium silicate according to mass ratio:
Phenolic resin=1: 0.2,1: 0.4,1: 0.6,1: 0.8,1: 1), be separately added into above-mentioned zirconium silicate colloidal sol, add at the same time
24.75g lithium molybdates are (according to quality than zirconium silicate: lithium molybdate=1: 3), after mixing, solution evaporates at 90 DEG C, obtains
Carbon black predecessor is wrapped up to zirconium silicate；
(3) above-mentioned zirconium silicate parcel carbon black predecessor is warming up to 950 DEG C of insulation 4h in nitrogen atmosphere with 5 DEG C/min,
Furnace cooling, obtains mixed powder；
(4) above-mentioned mixed powder through pickling, washing it is each 2 times to remove fused salt and unnecessary silica, then in air gas
800 DEG C of insulation 1h are warming up to remove unnecessary not wrapped carbon black with 3 DEG C/min in atmosphere, furnace cooling, that is, obtain silicic acid
Zirconium wraps up carbon black colorant.
The XRD test results of Fig. 1 show that the present embodiment obtains the parcel carbon black colorant that principal crystalline phase is zirconium silicate；And silicon
Sour zirconium grain development is good, its particle diameter is less than 5 μm (see Fig. 2,2~5 μm), and grain size is uniform.
The CIE L of Fig. 3*a*b*Curve shows that zirconium silicate manufactured in the present embodiment wraps up carbon black colorant, its L*Respectively
36.01、35.17、30.42、28.34、32.32；To be not added with the occlusion pigment of fused salt as a comparison case, identical experiment condition
Its lower L*Respectively 50.06,49.94,57.74,65.89,67.13.Show the present embodiment zirconium silicate parcel carbon black colorant its
Black color generation property is better than comparative example (L*The black colour generation ability of the lower colorant of value is better), there is excellent black colour generation to imitate
Fruit.
Embodiment two：
The method that a kind of fused salt auxiliary of the present embodiment prepares zirconium silicate parcel carbon black colorant, its step are as follows：
(1) 0.7mL zirconium-n-propylates and 0.5mL silane coupling agent aminopropyl triethoxysilanes are dissolved in 45mL normal propyl alcohols
In, the silicic acid zirconium solution that concentration is 0.05mol/L is formed, then adds 0.014g sodium fluorides (for the 3.5wt% of zirconium silicate), is mixed
Solvent thermal reaction 24h obtains zirconium silicate colloidal sol at a temperature of 75 DEG C after closing uniformly；
(2) 0.04g colour carbon blacks are weighed (according to quality than zirconium silicate: colour carbon black=1: 0.1), add above-mentioned zirconium silicate
In colloidal sol, while 0.412g tungstate lithiums are added (according to quality than zirconium silicate: tungstate lithium=1: 1), after mixing, at 130 DEG C
Solution is evaporated, obtains zirconium silicate parcel carbon black predecessor；
(3) above-mentioned zirconium silicate parcel carbon black predecessor is warming up to 850 DEG C of insulation 3h in nitrogen atmosphere with 4 DEG C/min,
Furnace cooling, obtains mixed powder；
(4) above-mentioned mixed powder through pickling, washing it is each 2 times to remove fused salt and unnecessary silica, then in air gas
800 DEG C of insulation 1h are warming up to remove unnecessary not wrapped carbon black with 3 DEG C/min in atmosphere, furnace cooling, that is, obtain silicic acid
Zirconium wraps up carbon black colorant.
The XRD test results of Fig. 4 show that the present embodiment obtains the parcel carbon black colorant that principal crystalline phase is zirconium silicate；And silicon
Sour zirconium grain development is good.The SEM of Fig. 5 the result shows that the occlusion pigment even grain size obtained is tiny, particle diameter for 0.5~
1μm.Using CIE L*a*b*Method is tested, and the zirconium silicate parcel carbon black colorant chromatic value of the present embodiment is L*=35.98, a*=
1.20、b*=3.59.
Embodiment three：
The method that a kind of fused salt auxiliary of the present embodiment prepares zirconium silicate parcel carbon black colorant, its step are as follows：
(1) eight water oxygen zirconium chlorides of 29.0g and 9.2mL non-hydrate sodium metasilicates are dissolved in 45mL distilled water, forming concentration is
The silicic acid zirconium solution of 2.0mol/L, then adds 1.16g magnesium fluorides (for the 7.0wt% of zirconium silicate), after mixing at 80 DEG C
At a temperature of hydro-thermal reaction 2h obtain zirconium silicate colloidal sol；
(2) weigh 8.25g sucrose (according to quality than zirconium silicate: sucrose=1: 0.5), add in above-mentioned zirconium silicate colloidal sol,
The composite fused salt of 16.50g sodium chloride and 16.50g potassium chloride composition is added at the same time (according to quality than zirconium silicate: sodium chloride: chlorination
Potassium=1: 1: 1), after mixing, solution evaporates at 120 DEG C, obtains zirconium silicate parcel carbon black predecessor；
(3) above-mentioned zirconium silicate parcel carbon black predecessor is warming up to 900 DEG C of insulation 3h in nitrogen atmosphere with 3 DEG C/min,
Furnace cooling, obtains mixed powder；
(4) above-mentioned mixed powder through pickling, washing it is each 2 times to remove fused salt and unnecessary silica, then in air gas
700 DEG C of insulation 4h are warming up to remove unnecessary not wrapped carbon black with 5 DEG C/min in atmosphere, furnace cooling, that is, obtain silicic acid
Zirconium wraps up carbon black colorant.
The XRD test results of Fig. 6 show that the present embodiment obtains the parcel carbon black colorant that principal crystalline phase is zirconium silicate.Using
CIE L*a*b*Method is tested, and the zirconium silicate parcel carbon black colorant chromatic value of the present embodiment is L*=31.71, a*=1.24, b*=
3.08。
Example IV：
The method that a kind of fused salt auxiliary of the present embodiment prepares zirconium silicate parcel carbon black colorant, its step are as follows：
(1) 3.7mL acetic acid zirconium and 7.1mL ethyl orthosilicates are dissolved in 45mL acetic acid, it is 0.7mol/L's to form concentration
Silicic acid zirconium solution, then adds 0.23g lithium chlorides (for the 4.0wt% of zirconium silicate), is heated after mixing at a temperature of 90 DEG C
Reaction 5h obtains zirconium silicate colloidal sol；
(2) 1.73g cotton fibers are weighed (according to quality than zirconium silicate: cotton fiber=1: 0.3), add above-mentioned zirconium silicate colloidal sol
In, while 34.65g sodium tungstates are added (according to quality than zirconium silicate: sodium tungstate=1: 6), after mixing, will be molten at 130 DEG C
Liquid evaporates, and obtains zirconium silicate parcel carbon black predecessor；
(3) above-mentioned zirconium silicate parcel carbon black predecessor is warming up to 950 DEG C of insulation 4h in nitrogen atmosphere with 5 DEG C/min,
Furnace cooling, obtains mixed powder；
(4) above-mentioned mixed powder through pickling, washing it is each 2 times to remove fused salt and unnecessary silica, then in air gas
800 DEG C of insulation 1h are warming up to remove unnecessary not wrapped carbon black with 3 DEG C/min in atmosphere, furnace cooling, that is, obtain silicic acid
Zirconium wraps up carbon black colorant.
The XRD test results of Fig. 7 show that the present embodiment obtains the parcel carbon black colorant that principal crystalline phase is zirconium silicate.Using
CIE L*a*b*Method is tested, and the zirconium silicate parcel carbon black colorant chromatic value of the present embodiment is L*=34.01, a*=1.72, b*=
3.23。
Claims (10)
1. a kind of method that fused salt auxiliary prepares zirconium silicate parcel carbon black colorant, it is characterised in that comprise the following steps：
(1) silicon source and zirconium source are dissolved in water or organic solvent according to stoichiometric ratio formed molar concentration for 0.05~
The silicic acid zirconium solution of 3.0mol/L, and mineralizer is added, after being uniformly mixed zirconium silicate colloidal sol is obtained through sol-gel process；
(2) carbon source and fused salt are added in the zirconium silicate colloidal sol, according to zirconium silicate described in mass ratio: carbon source: fused salt=1:
0.01~1: 1~6, solution is evaporated at a temperature of 80~150 DEG C after mixing, obtains zirconium silicate parcel carbon black forerunner
Thing；
(3) zirconium silicate parcel carbon black predecessor is heat-treated under nonoxidizing atmosphere, furnace cooling, obtains mixed powder
Body；
(4) mixed powder is through pickling, washing, and after being heat-treated under oxidizing atmosphere, furnace cooling, that is, obtain zirconium silicate
Wrap up carbon black colorant.
2. the method that fused salt auxiliary according to claim 1 prepares zirconium silicate parcel carbon black colorant, it is characterised in that：It is described
In step (1), the organic solvent is ethanol, normal propyl alcohol or acetic acid；The sol-gel process is directly heats or solvent
Thermal response, temperature are 70~100 DEG C, and the reaction time is 1~24h.
3. the method that fused salt auxiliary according to claim 1 prepares zirconium silicate parcel carbon black colorant, it is characterised in that：It is described
The dosage of mineralizer is 1.5~7.0wt% of zirconium silicate.
4. the method that fused salt auxiliary according to claim 1 prepares zirconium silicate parcel carbon black colorant, it is characterised in that：It is described
Silicon source is ethyl orthosilicate, silicon tetrachloride, waterglass, silane coupling agent or sodium metasilicate；The zirconium source is zirconium chloride, oxygen chlorine
Change zirconium, acetic acid zirconium, zirconium sulfate, zirconium nitrate, zirconium-n-propylate or zirconium iso-propoxide.
5. the method that the fused salt auxiliary according to claim 1 or 3 prepares zirconium silicate parcel carbon black colorant, it is characterised in that：
The mineralizer is lithium fluoride, magnesium fluoride, sodium fluoride, calcirm-fluoride or lithium chloride.
6. the method that fused salt auxiliary according to claim 1 prepares zirconium silicate parcel carbon black colorant, it is characterised in that：It is described
Carbon source is carbon black powder, phenolic resin, plant fiber, sucrose, fructose, glucose or starch.
7. the method that fused salt auxiliary according to claim 1 prepares zirconium silicate parcel carbon black colorant, it is characterised in that：It is described
Fused salt is the composite fused salt that alkali tungstates, alkali metal molybdate, one kind in alkali metal chloride or its combination are formed；Institute
It is respectively lithium, sodium, potassium element to state alkali metal.
8. the method that fused salt auxiliary according to claim 7 prepares zirconium silicate parcel carbon black colorant, it is characterised in that：It is described
When composite fused salt is made of two kinds of fused salts, according to mass ratio, its ratio be 1~9: 1~9.
9. the method that fused salt auxiliary according to claim 1 prepares zirconium silicate parcel carbon black colorant, it is characterised in that：This hair
In the bright step (3), heat treating regime is warming up to 800~1050 DEG C of insulations 1 for 3~5 DEG C/min under the nonoxidizing atmosphere
~4h；In the step (4), heat treating regime is warming up to 700~900 DEG C of insulations 1 for 3~5 DEG C/min under the oxidizing atmosphere
~4h.
10. product made from the method for zirconium silicate parcel carbon black colorant is prepared using one of the claim 1-9 fused salt auxiliary,
It is characterized in that：The colorant product appearance and size is uniformly tiny, and particle diameter is 0.5~5 μm.
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| CN115490238A (en) * | 2022-09-13 | 2022-12-20 | 泉州师范学院 | SiO (silicon dioxide) 2 Aerogel/carbon composite porous powder material and preparation method thereof |
| CN115536439A (en) * | 2022-09-27 | 2022-12-30 | 广东简一(集团)陶瓷有限公司 | One-time high-temperature fired noctilucent ceramic tile and preparation method thereof |
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Application publication date: 20180420 |