CN105647243B - It is a kind of that carbon black preparation method and its obtained product are wrapped up based on the mesoporous zirconium silicate collapsed - Google Patents
It is a kind of that carbon black preparation method and its obtained product are wrapped up based on the mesoporous zirconium silicate collapsed Download PDFInfo
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- CN105647243B CN105647243B CN201511019185.1A CN201511019185A CN105647243B CN 105647243 B CN105647243 B CN 105647243B CN 201511019185 A CN201511019185 A CN 201511019185A CN 105647243 B CN105647243 B CN 105647243B
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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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- 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/62—L* (lightness axis)
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Abstract
Carbon black preparation method is wrapped up based on the mesoporous zirconium silicate collapsed the invention discloses a kind of, is prepared to obtain template zirconia sol using inorganic zirconium salts and template as raw material, template carbonization is obtained a powder by pre-burning after gelation；After powder adds Ludox mixing, secondary powder is obtained through gelation；The secondary powder is calcined under nonoxidizing atmosphere, that is, obtains zirconium silicate parcel carbon black colorant.Product made from above-mentioned preparation method is utilized in addition, also disclosing.The present invention realizes that the fine and close of carbon black wraps up using collapsing for meso-hole structure, the preparation that carbon black is wrapped up for zirconium silicate provides new approach, encapsulation ratio is not only effectively increased, and the subsequent oxidation problem of carbon black can be prevented, so as to which the zirconium silicate obtained in obvious black wraps up carbon black products.
Description
Technical field
The present invention relates to ceramic pigment technical field, more particularly to the preparation method and its system of a kind of zirconium silicate parcel carbon black
The product obtained.
Background technology
At present, inkjet printing has turned into the important technology of building ceramic decoration, and black is the ceramic ink that must be used
One of, the black ceramic colorant as ceramic ink needs to have less particle diameter to avoid blocking shower nozzle.Prior art black
Ceramic pigment is the spinel oxides containing elements such as Fe, Co, Mn using Solid phase synthesis, and these have what is necessarily matched
When ion is in ligand field of different shapes, ligand-field effect is generated, complementary light absorbs are produced to light and realized black
Color.But when this black ceramic colorant is ground to suitable for preparing the granularity needed for ceramic ink, spinel-type oxygen can be caused
Compound structural damage, it is final to influence black colouring effect so as to which the absorption influenceed to light causes color deviation.
Carbon black has pure black, but easily aoxidizes at high operating temperatures, it is therefore desirable to wrapped up using zirconium silicate,
The coated carbon black obtained just can serve as ceramic pigment.But the key problem for preparing zirconium silicate parcel carbon black colorant is zirconium silicate
It is not high to the encapsulation ratio of carbon black, integument is not fine and close, carbon black is not spontaneously wet out by water, is difficult to disperse in addition, so as to influence to wrap up efficiency,
So just cause current product to be typically only capable to obtain grey (the brightness value L* in colourity is more than 30).Therefore, prior art master
To be solved in terms of following two：First, the formation condition by controlling zirconium silicate, is wrapped up with obtaining fine and close zirconium silicate
Layer；Second, using organic matter precursor such as powdered thermosetting phenolic resin as raw material, carbon black is formed by fabricated in situ, to solve charcoal
It is black to be difficult to the problem of dispersed.Although prior art improves parcel problem to a certain extent, wrapped up for zirconium silicate
The formation of layer is required to add fluoride-mineralization agent etc., not only have impact on the black level of colorant, and the cause of colorant integument
Close property and encapsulation ratio are still undesirable, and encapsulation ratio highest only has 63%, show that preparation-obtained zirconium silicate parcel carbon black is still
Grey, have no the preparation problem for efficiently solving black parcel carbon black colorant.
Mesoporous material refers to a polyporous materials of the aperture between 2~50nm, has high specific surface area, regular
Pore passage structure, narrow pore-size distribution, pore size continuously adjustabe the features such as.The meso-hole structure of mesoporous material mainly uses mould
Plate agent method synthesizes, and by calcining or cleaning after template agent removing forms meso-hole structure.But when calcining heat is higher
(600 DEG C of ＞), meso-hole structure will collapse and become fine and close, lose porous property.Therefore, at present on mesoporous material, it grinds
The emphasis studied carefully is how to control its structure still to keep meso-hole structure at higher temperatures.And on by destroying mesoporous knot
Structure, i.e. collapsing to synthesize the method for parcel ceramic pigment using meso-hole structure, there is no report at present.
The content of the invention
Charcoal is wrapped up based on the mesoporous zirconium silicate collapsed it is an object of the invention to overcome the deficiencies of the prior art and provide a kind of
Black preparation method, realize that the fine and close of carbon black wraps up using collapsing for meso-hole structure, and obtain and wrapped up in the zirconium silicate of obvious black
Carbon black, the preparation that carbon black is wrapped up for zirconium silicate provide new approach.Another object of the present invention is to provide to utilize above-mentioned preparation
Product made from method.
The purpose of the present invention is achieved by the following technical programs：
A kind of zirconium silicate parcel carbon black preparation method for being collapsed based on mesoporous provided by the invention is as follows, with inorganic zirconium salts and
Template is that raw material is prepared to obtain template-zirconia sol, obtains template carbonization by pre-burning after gelation
Obtain a powder；After powder adds Ludox mixing, secondary powder is obtained through gelation；The secondary powder exists
Calcined under nonoxidizing atmosphere, that is, obtain zirconium silicate parcel carbon black colorant.
The present invention, using sol-gel process, utilizes organic formwork agent using inorganic zirconium salts, template and Ludox as raw material
Form mesoporous zirconium silicate.By being calcined under nonoxidizing atmosphere, organic formwork agent anoxic is cracked into carbon black, and is collapsed mesoporous
Structure is closed, so as to obtain zirconium silicate parcel carbon black colorant.
Preparation method of the present invention specifically comprises the following steps：
(1) template-zirconia sol is prepared
According to quality than template: zirconium oxide=0.01~0.70: 1, inorganic zirconium salts and template are dissolved in the water, added
Enter weak caustic solution, preparation obtains containing Zr4+0.4~0.8mol/L template-zirconia sol；
(2) template-zirconium oxide sol-gel
After the template-zirconia sol is by heated gel, dry template-zirconium oxide gel is obtained；
(3) carbonization of template
The template of the drying-zirconium oxide gel is subjected to pre-burning under nonoxidizing atmosphere, calcining heat is 300~
350 DEG C, it is incubated 1~2h；After pre-burning a powder is obtained through grinding；
(4) introducing of silica
According to quality than silica: zirconium oxide=1.1~2.0: 1, by a powder under ultrasound or stirring condition
Add in Ludox, secondary powder is obtained through gelation and after drying；
(5) meso-hole structure collapse and the preparation of zirconium silicate integument
The secondary powder is calcined under nonoxidizing atmosphere, and calcining heat is 1000~1250 DEG C, is incubated 10~120min；
Zirconium silicate parcel carbon black colorant is obtained after removing the carbon black not wrapped up.
Further, inorganic zirconium salts of the present invention are zirconium oxychloride (ZrOCl2·8H2O), zirconium nitrate (Zr (NO3)4·
5H2O), zirconium chloride (ZrCl4)；The weak base is weak aqua ammonia, hexa, monoethanolamine.The template is cetyl
Ammonium bromide, dodecyl sodium sulfate, triblock polymer P123, triblock polymer F127.
Further, the gel of step (2) of the present invention turns to two-stage drying process, i.e., first by template-oxidation
Zirconium colloidal sol is dried in g., jelly-like at a temperature of 40~60 DEG C and obtains wet gel, and then is dried at a temperature of 100~150 DEG C,
Obtain dry template-zirconium oxide gel.Or the gel of the step (2) turns to rapid heating process, i.e., by template
Agent-zirconia sol is placed in tray, gelation, drying at a temperature of 100~150 DEG C, obtains dry template-zirconium oxide
Gel.
Using above-mentioned based on product, its brightness value L*=20 made from the mesoporous zirconium silicate parcel carbon black preparation method collapsed
~29.
The invention has the advantages that：
(1) present invention provides new approach for the preparation of zirconium silicate parcel carbon black colorant.Utilize template, zirconium source, silicon
Source raw material forms meso-hole structure zirconium silicate, and carbon black derives from the cracking of template, caved in by calcining meso-hole structure and incite somebody to action
Carbon black pellet is enclosed within original meso-hole structure, wraps up carbon black colorant so as to obtain the fine and close zirconium silicate of parcel, product is in pure
Positive black, its brightness value L* are 20~29.
(2) present invention prepares zirconium silicate using sol-gel process, and cost of material is low, and without cleaning in preparation process,
So as to effectively reduce the cost of zirconium silicate occlusion pigment.
(3) present invention effectively increases the mixing of silica and zirconium oxide using sol-gel process, without adding fluoride
Mineralizer etc. promotes the generation of zirconium silicate, and what the colorant blackness caused by thus avoid fluoride-mineralization agent etc. reduced asks
Topic.
(4) carbon black of the present invention derives from the cracking (about 200~450 DEG C of cracking temperature) of template, and template can be with
The form of molecular level is dispersed in zirconium silicate, is not spontaneously wet out by water caused reunion so as to effectively prevent carbon black, is solved well
The problem of encapsulation ratio of having determined is not high.
(5) present invention collapsing and (typically just occurring by 600 DEG C of calcinings and cave in) using meso-hole structure, will can crack
Tiny carbon black pellet be enclosed within original meso-hole structure, meso-hole structure not only constitutes dense protective layer, and can
Ensure that carbon black pellet is wrapped to greatest extent, not only effectively increase encapsulation ratio, and the subsequent oxidation of carbon black can be prevented
Problem.
Brief description of the drawings
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail：
Fig. 1 is the transmission electron microscope photo of the zirconium silicate parcel carbon black colorant prepared by the embodiment of the present invention one.
Embodiment
Embodiment one：
The present embodiment is a kind of to wrap up carbon black preparation method based on the mesoporous zirconium silicate collapsed, and its step is as follows：
(1) preparation of template-zirconia sol
By 38.7gZrOCl2It is dissolved in 6g triblock polymer P123 templates in 100g deionized waters and obtains containing P123
Zirconyl chloride solution, 13.46g hexas are dissolved in 100g deionized waters and obtain weak caustic solution；Will be above-mentioned weak
Aqueous slkali is slowly dropped into the zirconyl chloride solution containing P123, and preparation obtains containing Zr4+0.6mol/L template-zirconium oxide is molten
Glue；
(2) template-zirconium oxide sol-gel
Template-zirconia sol is placed in baking oven, is dried at a temperature of 50 DEG C in g., jelly-like and obtains wet gel；
And then be warming up to 110 DEG C and be dried, obtain dry template-zirconium oxide gel；
(3) carbonization of template
Dry template-zirconium oxide gel is put into Muffle furnace, is buried using graphite and burns into row pre-burning, calcining heat is
300 DEG C, it is incubated 2h；Then ball milling 4h and obtain a powder；
(4) introducing of silica
According to quality than silica: zirconium oxide=1.5: 1, a powder is added into concentration under ultrasound or stirring condition is
In 30wt% Ludox, it is subsequently placed in baking oven and secondary powder is obtained through gelation and after drying；
(5) preparation of zirconium silicate integument
Secondary powder is put into Muffle furnace, in high-purity N2Calcined under protection, calcining heat is 1100 DEG C, insulation
10min；Then 900 DEG C are cooled to, closes N2, the carbon black that 120min is not wrapped up to remove is incubated, silicic acid is obtained with stove cooling
Zirconium wraps up carbon black colorant.
As shown in figure 1, the meso-hole structure that lower section micellelike (shown in arrow) is formed by P123 micellas, P123 crack to be formed
Carbon black be closed wherein.
Use the brightness value L*=27.8 of the obtained zirconium silicate parcel carbon black colorant of colorimeter measurement.
Embodiment two：
The present embodiment is a kind of to wrap up carbon black preparation method based on the mesoporous zirconium silicate collapsed, exists with the difference of embodiment one
In：According to quality than silica in step (4): zirconium oxide=2.0: 1；Step (5) high-purity N2The lower calcining heat of protection is 1200
℃。
Use the brightness value L*=25.01 of the obtained zirconium silicate parcel carbon black colorant of colorimeter measurement.
Embodiment three：
The present embodiment is a kind of to wrap up carbon black preparation method based on the mesoporous zirconium silicate collapsed, exists with the difference of embodiment one
In：Template is 10g cetyl ammonium bromides in step (1).
Use the brightness value L*=29.21 of the obtained zirconium silicate parcel carbon black colorant of colorimeter measurement.
Example IV：
The present embodiment is a kind of to wrap up carbon black preparation method based on the mesoporous zirconium silicate collapsed, exists with the difference of embodiment one
In：Template-zirconia sol is placed in tray by step in (2), is put into 110 DEG C of baking ovens by quickly heating and gel
Change, after drying, obtain dry template-zirconium oxide gel；High-purity N in step (5)2The lower calcining heat of protection is 1200 DEG C.
Use the brightness value L*=23.8 of the obtained zirconium silicate parcel carbon black colorant of colorimeter measurement.
Claims (8)
1. a kind of wrap up carbon black preparation method based on the mesoporous zirconium silicate collapsed, it is characterised in that：With inorganic zirconium salts and template
Prepared to obtain template-zirconia sol for raw material, wherein, the template is cetyl ammonium bromide, dodecyl
Sodium sulfonate, triblock polymer P123, triblock polymer F127；Template-the zirconia sol passes through after gelation
Pre-burning makes template be carbonized and obtains a powder；After powder adds Ludox mixing, two are obtained through gelation
Secondary powder；The secondary powder is calcined under nonoxidizing atmosphere, that is, obtains zirconium silicate parcel carbon black colorant.
2. according to claim 1 wrap up carbon black preparation method based on the mesoporous zirconium silicate collapsed, it is characterised in that including
Following steps：
(1) template-zirconia sol is prepared
According to quality than template: zirconium oxide=0.01~0.70: 1, inorganic zirconium salts and template are dissolved in the water, added weak
Aqueous slkali, preparation obtain containing Zr4+0.4~0.8mol/L template-zirconia sol；
(2) template-zirconium oxide sol-gel
After the template-zirconia sol is by heated gel, dry template-zirconium oxide gel is obtained；
(3) carbonization of template
The template of the drying-zirconium oxide gel is subjected to pre-burning under nonoxidizing atmosphere, calcining heat is 300~350 DEG C,
It is incubated 1~2h；After pre-burning a powder is obtained through grinding；
(4) introducing of silica
According to quality than silica: zirconium oxide=1.1~2.0: 1, a powder is added under ultrasound or stirring condition
In Ludox, secondary powder is obtained through gelation and after drying；
(5) meso-hole structure collapse and the preparation of zirconium silicate integument
The secondary powder is calcined under nonoxidizing atmosphere, and calcining heat is 1000~1250 DEG C, is incubated 10~120min；Remove
Zirconium silicate parcel carbon black colorant is obtained after the carbon black not wrapped up.
3. according to claim 1 or 2 wrap up carbon black preparation method based on the mesoporous zirconium silicate collapsed, it is characterised in that：
The inorganic zirconium salts are zirconium oxychloride, zirconium nitrate, zirconium chloride.
4. according to claim 2 wrap up carbon black preparation method based on the mesoporous zirconium silicate collapsed, it is characterised in that：It is described
Weak base is weak aqua ammonia, hexa, monoethanolamine in step (1).
5. according to claim 2 wrap up carbon black preparation method based on the mesoporous zirconium silicate collapsed, it is characterised in that：It is described
The gel of step (2) turns to two-stage drying process, i.e., is first dried to template-zirconia sol at a temperature of 40~60 DEG C
Wet gel is obtained in g., jelly-like, and then is dried at a temperature of 100~150 DEG C, obtains dry template-zirconium oxide gel.
6. according to claim 2 wrap up carbon black preparation method based on the mesoporous zirconium silicate collapsed, it is characterised in that：It is described
The gel of step (2) turns to rapid heating process, i.e., template-zirconia sol is placed in tray, in 100~150 DEG C of temperature
Degree lower gelation, drying, obtain dry template-zirconium oxide gel.
7. product made from carbon black preparation method is wrapped up based on the mesoporous zirconium silicate collapsed using described in one of claim 1-6.
8. according to claim 7 based on product made from the mesoporous zirconium silicate parcel carbon black preparation method collapsed, it is special
Sign is：Brightness value L*=20~29 of the product.
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| CN114058083B (en) * | 2021-11-29 | 2023-06-20 | 江西广源化工有限责任公司 | Zirconium-based magnesium hydroxide and preparation method and application thereof |
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| CN103193511B (en) * | 2013-04-25 | 2014-11-05 | 景德镇陶瓷学院 | Preparation method of zirconium silicate wrapped ceramic pigment |
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