CN107325586B - A kind of method of soft mechanical force and chemical assisted Solid-state method titania type titanium yellow ceramic pigment - Google Patents
A kind of method of soft mechanical force and chemical assisted Solid-state method titania type titanium yellow ceramic pigment Download PDFInfo
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- CN107325586B CN107325586B CN201710455152.4A CN201710455152A CN107325586B CN 107325586 B CN107325586 B CN 107325586B CN 201710455152 A CN201710455152 A CN 201710455152A CN 107325586 B CN107325586 B CN 107325586B
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- 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 belongs to technical field of ceramic material, disclose a kind of method of soft mechanical force and chemical assisted Solid-state method titania type titanium yellow ceramic pigment.Titanium dioxide, nickel salt and antimony oxide are distributed in deionized water, it then is 500~4000r/min in revolving speed by medium stirring mill, abrasive media filling rate is 60~80vol.%, abrasive media is having a size of 0.1~0.8mm, soft mechanical force and chemical processing is carried out under conditions of 10~60min of milling time, presoma is obtained, is sintered then at 900~1200 DEG C, obtains rutile-type titanium yellow ceramic pigment.Titanium yellow ceramic pigment prepared by the present invention is in Rutile structure, and chemical property is stable and high temperature resistance is good；Pure color simultaneously, yellow value degree, brightness value are higher；Sintering temperature can at least reduce by 100 DEG C compared with conventional solid-state method, and less energy consumption has broad application prospects.
Description
Technical field
The invention belongs to technical field of ceramic material, and in particular to a kind of soft mechanical force and chemical assisted Solid-state method synthesis golden red
The method of stone-type titanium yellow ceramic pigment.
Background technique
Inorganic color has good thermal stability and chemical stability, is widely used in multiple industrial circles, especially
It is ceramic industry.The raw material of conventional yellow ceramic pigment contains the heavy metal elements such as Cd, Cr, Pb more, is easy to seep in use process
Out, environmental pollution is caused, human health is influenced；It is much about environmentally friendly yellow ceramic pigment in existing patent
Preparation method.Chinese patent CN104892030A discloses " preparation method of a kind of nanometer of praseodymium yellow ceramic pigment " using colloidal sol
Gel method is prepared for the presoma of pr-yellow material, handles 1~2h by ball mill grinding, then be sintered to obtain environmental-friendly
Pr-yellow material.Contain Rare Earth Elements of Praseodymium in the raw material of the praseodymium yellow ceramic pigment of the method preparation, preparation cost is high, and preparation process
Complexity is unfavorable for large-scale application.
Rutile-type titanium yellow ceramic pigment enters TiO using Ni, Sb ion doping2The method system of rutile crystalline structure
Standby, former material is cheap.Rutile structure has preferable chemical stability and high temperature resistance.Ni, Sb ion doping into
Enter in rutile crystal, be not easy to ooze out in use, therefore, rutile-type titanium yellow ceramic pigment is a kind of environment friend
Good type ceramic pigment.Currently, deficiency existing for rutile-type titanium yellow ceramic pigment is mainly shown as that yellow value degree is lower and is biased to
Yellowish green tone, (M.Dondi, G.Cruciani, F.matteucci, et al., The the role of such as lightness deficiency
counterions(Mo,Nb,Sb,W)in Cr-,Mn-,Ni-and V-doped rutile ceramic pigments:part
2.colour and technological properties,Cream.Int.32(4)(2006)393-405).Therefore, now
Urgently to be resolved is the chromophoric characteristic that rutile-type titanium yellow ceramic pigment is improved using inexpensive effective ways, and acquisition becomes clear pure
Yellow titanium yellow ceramic pigment.
It prepares inorganic ceramic colorant and generallys use solid phase method, sol-gal process and chemical precipitation method etc..Sol-gal process
It is smaller with chemical precipitation method complex process, higher cost, yield.Traditional solid phase method simple process, yield is big, but energy consumption
Height, product purity is low, partial size is big.Mechanochemical method as a kind of simple process and the few method of energy consumption receive it is more and more
Concern.Chinese patent CN1699271 is disclosed " with the method for preparing high-purity mullite at low temperature by mechanochemical process ", using row
Celestial body grinding machine or vibromill carry out grinding pretreatment to raw material, are sintered at 1150~1450 DEG C, and obtaining purity is 95~98%
Mullite, calcination temperature is reduced, to save the energy.But planetary ball mill or vibromill energy density are low, required grinding
It is longer to handle the time.
Summary of the invention
In place of the above shortcoming and defect of the existing technology, the primary purpose of the present invention is that providing a kind of soft machine
The method of tool power chemistry assisted Solid-state method titania type titanium yellow ceramic pigment.This method is at low cost, environmentally friendly, institute
Ceramic pigment yellow value degree is high, yellow is pure, brightness value is high.
A further object of the present invention is to provide one kind to pass through rutile-type titanium yellow ceramic pigment obtained by the above method.
The object of the invention is achieved through the following technical solutions:
A kind of method of soft mechanical force and chemical assisted Solid-state method titania type titanium yellow ceramic pigment, including walk as follows
It is rapid:
(1) titanium dioxide, nickel salt and antimony oxide are add to deionized water, add dispersing agent and is dispersed with stirring
It is even, obtain suspension；
(2) suspension of step (1) is added in medium stirring mill and carries out soft mechanical force and chemical processing, revolving speed control is
500~4000r/min, abrasive media filling rate are 60~80vol.%, and abrasive media size Control is 0.1~0.8mm, grinding
10~60min of time obtains finely dispersed suspension；
(3) suspension obtained by step (2) be dry, pulverize into sieving, obtains rutile-type titanium yellow ceramic pigment presoma
Powder；
(4) precursor powder obtained by step (3) is warming up to 900~1200 DEG C of heat preservation sinterings, Temperature fall obtains described
Rutile-type titanium yellow ceramic pigment.
Preferably, the additional proportion of titanium dioxide described in step (1), nickel salt and antimony oxide are as follows: so that adulterate from
The molar content of sub- Ni is 1~5mol.% and the molar ratio of Ni, Sb ion is Ni:Sb=1:2.
Preferably, nickel salt described in step (1) refers to nickel nitrate or nickel sulfate.
Preferably, dispersing agent described in step (1) is WF-211 or AD-8030, the dosage of dispersing agent is 1~
5wt.%.
Preferably, the solid content of suspension described in step (1) is 20~30wt.%.
Preferably, drying described in step (3) refers in 90~110 DEG C of dry 8~12h.
Preferably, the rate of heating described in step (4) is 5~20 DEG C/min, time of the heat preservation sintering is 0.5~
2h。
A kind of rutile-type titanium yellow ceramic pigment, is prepared by the above method.
Compared with the existing technology, method of the invention have the following advantages that and the utility model has the advantages that
(1) present invention is using soft mechanical force and chemical to the raw material for titania type titanium yellow ceramic pigment
Activation is learned, then is sintered to obtain product using solid phase method.With the colorant without the processing solid phase method sintering synthesis of soft mechanical force and chemical
It compares, is substantially reduced using the solid phase sintering temperature of the presoma of the method preparation, the rutile-type titanium yellow ceramic pigment of acquisition
Expect that yellow chrominance is pure, hair color effect is good, is with a wide range of applications.
(2) preparation process of the invention is simple, mechanical lapping short processing time, the more traditional solid phase method of sintering temperature
(1200~1300 DEG C) reduce by 100 DEG C, greatly reduce energy consumption, no waste discharge, yield are big, are adapted to industrial solid
Phase preparation method.
(3) different from using conventional planet ball mill (general Ball-milling Time need to be up to for 24 hours), the grinding machine that the present invention selects is
Medium stirring mill, capacity usage ratio are high, only need 10~60min that can be effectively reduced the burning of synthesis colorant raw material milled processed
Junction temperature.
(4) the rutile-type titanium yellow ceramic pigment chromatic value of the method for the present invention preparation is L*=82.08, a*=0.49, b*
=62.74, particle size is 200~300nm, is that a kind of yellow is pure and in the lesser environmentally friendly nothing of bright yellow hue, grain graininess
The ceramic pigment of poison can be widely applied in actual production life.
Detailed description of the invention
Fig. 1 is the X-ray powder diffraction figure of rutile-type titanium yellow ceramic pigment prepared by the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of rutile-type titanium yellow ceramic pigment prepared by the present invention.
Fig. 3 is that the ultraviolet-visible light splitting of rutile-type titanium yellow ceramic pigment prepared by the present invention absorbs figure.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
A kind of method of the soft mechanical force and chemical assisted Solid-state method titania type titanium yellow ceramic pigment of the present embodiment,
Specific step is as follows:
(1) titanium dioxide of 33.988g, the antimony oxide of 1.933g and the six water nickel nitrates of 4.080g are weighed, it will
It is added to 120g deionized water, and 0.4g WF-211 dispersing agent is added dropwise, with glass bar stir solid content is the outstanding of 25wt.%
Supernatant liquid.
(2) suspension described in step (1) is added in horizontal media Ball-stirring mill, high speed grinding handles 30min, revolving speed control
It is made as 1995r/min, abrasive media is 80vol.% having a size of 0.1mm, abrasive media filling rate, obtains finely dispersed suspension
Liquid.
(3) step (2) resulting suspension is fitted into the uncovered beaker of 500mL, and be put into constant temperature oven at 110 DEG C
Lower dry 8h obtains rutile-type titanium yellow colorant presoma, it crushed 160 meshes with mortar grinder and obtain precursor powder.
(4) precursor powder obtained in step (3) is packed into crucible, is placed in Muffle furnace, by 10 DEG C of temperature programmed control/
Min rises to 1100 DEG C, keeps the temperature 1h, is down to room temperature naturally then to get rutile-type titanium yellow ceramic pigment.
Embodiment 2
A kind of method of the soft mechanical force and chemical assisted Solid-state method titania type titanium yellow ceramic pigment of the present embodiment,
Specific step is as follows:
(1) titanium dioxide of 42.485g, the antimony oxide of 2.416g and the six water nickel nitrates of 5.099g are weighed, it will
It is added to 200g deionized water, and 0.5g WF-211 dispersing agent is added dropwise, stir solid content be 20wt.% suspension.
(2) suspension described in step (1) is added in vertical media Ball-stirring mill, high speed grinding handles 10min, revolving speed control
It is made as 2500r/min, abrasive media size Control is 0.3mm, and abrasive media filling rate is 75vol.%, is obtained finely dispersed
Suspension.
(3) step (2) resulting suspension is fitted into the uncovered beaker of 500mL, and be put into constant temperature oven at 90 DEG C
Lower dry 12h obtains rutile-type titanium yellow ceramic pigment presoma, it crushed 160 meshes with mortar grinder and obtain forerunner
Body powder.
(4) precursor powder obtained in step (3) is packed into crucible, is placed in Muffle furnace, by 5 DEG C of temperature programmed control/
Min rises to 900 DEG C, keeps the temperature 2h, is down to room temperature naturally then to get rutile-type titanium yellow ceramic pigment.
Embodiment 3
A kind of method of the soft mechanical force and chemical assisted Solid-state method titania type titanium yellow ceramic pigment of the present embodiment,
Specific step is as follows:
(1) titanium dioxide of 85.365g, the antimony oxide of 1.732g and the nickel sulfate of 2.903g are weighed, by itself plus
Enter to 210g deionized water, 0.9g AD-8030 dispersing agent be added dropwise, stir solid content be 30wt.% suspension.
(2) suspension described in step (1) is added in horizontal media Ball-stirring mill, high speed grinding handles 60min, revolving speed control
It is made as 1500r/min, abrasive media is 60vol.% having a size of 0.8mm, abrasive media filling rate, obtains finely dispersed suspension
Liquid.
(3) step (2) resulting suspension is fitted into the uncovered beaker of 500mL, and be put into constant temperature oven at 100 DEG C
Lower dry 10h obtains rutile-type titanium yellow colorant presoma, it crushed 160 meshes with mortar grinder and obtain precursor
End.
(4) precursor powder obtained in step (3) is packed into crucible, is placed in Muffle furnace, by 20 DEG C of temperature programmed control/
Min rises to 1100 DEG C, keeps the temperature 0.5h, is down to room temperature naturally then to get rutile-type titanium yellow ceramic pigment.
Titanium yellow ceramic pigment performance prepared by the present invention is as follows:
Fig. 1 is the X-ray powder diffraction pattern of the titanium yellow ceramic pigment of preparation.As can be seen that the titanium yellow pottery of preparation
Porcelain color is pure rutile phase, without other miscellaneous phases.Illustrate that Ni, Sb ion are fully doped to enter in Rutile Type structure, will not seep
It causes damages out to environment and human body.
Fig. 2 is the scanning electron microscope (SEM) photograph of the titanium yellow ceramic pigment of preparation.As shown, the titanium yellow ceramic pigment of preparation is in
Spherical or ellipsoid like structure, grain diameter are 200~300nm.
Fig. 3 is that the ultraviolet-visible of the titanium yellow ceramic pigment of preparation divides optical absorption map.As shown, the titanium nickel of preparation
Yellow ceramic pigment has biggish absorption peak in 380~560nm, it is seen that titanium yellow ceramic pigment is in preferable yellow.
Table 1 is the chromatic value of titanium yellow ceramic pigment in the titanium yellow ceramic pigment and correlative study of preparation.
Table 1
Titanium yellow ceramic pigment (L*=82.08, a*=0.49, b*=prepared by the present invention it can be seen from 1 result of table
62.74) the rutile-type titanium yellow ceramic pigment of yellow value degree and brightness value relative to other research preparations[1](L*=79, a*
=-3, b*=50) there is apparent raising, and yellow tone is more pure.([1]M.Dondi,G.Cruciani,
F.matteucci,et al.,The role of counterions(Mo,Nb,Sb,W)in Cr-,Mn-,Ni-and V-
doped rutile ceramic pigments:part 2.colour and technological properties,
Cream.Int.32(4)(2006)393-405)。
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (6)
1. a kind of method of soft mechanical force and chemical assisted Solid-state method titania type titanium yellow ceramic pigment, it is characterised in that packet
Include following steps:
(1) titanium dioxide, nickel salt and antimony oxide are add to deionized water, add dispersing agent and is dispersed with stirring uniformly,
Obtain suspension；
(2) suspension of step (1) is added in medium stirring mill and carries out soft mechanical force and chemical processing, revolving speed control is 500
~4000r/min, abrasive media filling rate are 60~80vol.%, and abrasive media size Control is 0.1~0.8mm, when grinding
Between 10~60min, obtain finely dispersed suspension；
(3) suspension obtained by step (2) be dry, pulverize into sieving, obtains rutile-type titanium yellow ceramic pigment precursor powder；
(4) precursor powder obtained by step (3) is warming up to 900~1200 DEG C of heat preservation sinterings, Temperature fall obtains the golden red
Stone-type titanium yellow ceramic pigment；
The additional proportion of titanium dioxide described in step (1), nickel salt and antimony oxide are as follows: so that Doped ions Ni's mole contains
Amount is Ni:Sb=1:2 for the molar ratio of 1~5% and Ni, Sb ion；
Nickel salt described in step (1) refers to nickel nitrate or nickel sulfate.
2. a kind of soft mechanical force and chemical assisted Solid-state method titania type titanium yellow ceramic pigment according to claim 1
Method, it is characterised in that: dispersing agent described in step (1) is WF-211 or AD-8030, the dosage of dispersing agent is 1~
5wt.%.
3. a kind of soft mechanical force and chemical assisted Solid-state method titania type titanium yellow ceramic pigment according to claim 1
Method, it is characterised in that: the solid content of suspension described in step (1) be 20~30wt.%.
4. a kind of soft mechanical force and chemical assisted Solid-state method titania type titanium yellow ceramic pigment according to claim 1
Method, it is characterised in that: drying described in step (3) refers in 90~110 DEG C of dry 8~12h.
5. a kind of soft mechanical force and chemical assisted Solid-state method titania type titanium yellow ceramic pigment according to claim 1
Method, it is characterised in that: the rate of heating described in step (4) is 5~20 DEG C/min, and the time of the heat preservation sintering is
0.5~2h.
6. a kind of rutile-type titanium yellow ceramic pigment, it is characterised in that: pass through the described in any item methods of Claims 1 to 5
It is prepared.
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