CN109233339A - In the production method of the zircon-vanadium blue pigment of green tune blue - Google Patents

In the production method of the zircon-vanadium blue pigment of green tune blue Download PDF

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CN109233339A
CN109233339A CN201811057008.6A CN201811057008A CN109233339A CN 109233339 A CN109233339 A CN 109233339A CN 201811057008 A CN201811057008 A CN 201811057008A CN 109233339 A CN109233339 A CN 109233339A
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zircon
vanadium
blue
electric
toner
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CN109233339B (en
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程诗忠
叶旦旺
李小毅
高鸿魁
李有成
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SANXIANG ADVANCED MATERIALS CO Ltd
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SANXIANG ADVANCED MATERIALS CO Ltd
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    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0009Pigments for ceramics
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0009Pigments for ceramics
    • C09C1/0012Pigments for ceramics containing zirconium and silicon
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/041Grinding
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/043Drying, calcination
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/66Hue (H*)

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Developing Agents For Electrophotography (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The present invention relates to ceramic pigment technical field, and it is an object of the present invention to provide a kind of production method of zircon-vanadium blue pigment, the production method of the zircon-vanadium blue pigment, granulation is handled after including the following steps: step 1, mixing fluxing agent, binder and the first toner;Step 2, by zircon sand and step 1 products therefrom, melting is handled at high temperature;Step 3 grinds the resulting electric-melting zirconia of step 2;Vanadium zirconium blue other raw materials are mixed and are ground with step 3 products therefrom by step 4, and cooling down obtains zircon-vanadium blue pigment after heating and calcining.The beneficial effects of the present invention are: by zircon sand and regulator high melt, and control after melting the content of toner and the granularity of electric-melting zirconia in electric-melting zirconia, finally plus other raw materials of Vanadium zirconium blue produce zircon-vanadium blue pigment, the zircon-vanadium blue pigment produced is in green tune blue, the demand of domestic ceramics and art ceramics industry to green tune blue is met, the color of ceramic is enriched.

Description

In the production method of the zircon-vanadium blue pigment of green tune blue
This case is with the applying date on May 08th, 2017, application No. is 201710315514.X, a kind of entitled " vanadium zirconium The divisional application that the patent of invention of the production method of blue " carries out for female case.
Technical field
The present invention relates to ceramic pigment technical field, in particular to a kind of production method of zircon-vanadium blue pigment.
Background technique
Zirconium ceramic pigment has the excellent performance that color development is bright-coloured, compatibility is good, uses to use in the common glaze of ceramics with base It is occupied an important position in colorant, wherein most common, maximum dosage is zirconium three primary colors: Vanadium zirconium blue, zirconium praseodymium yellow, zirconium iron pink, Principal crystalline phase is zirconium silicate, is generated at high temperature by zirconium oxide and quartz.The vanadium that domestic ceramics and art ceramics industry use at present Zirconium blue is all biased to green tone blue, and the zircon-vanadium blue pigment of common electric-melting zirconia production is in dark tune blue, makes green blue The hair color effect of tone is undesirable, is not able to satisfy domestic ceramics and art ceramics industry answering to the zircon-vanadium blue pigment of green tune blue With requiring.Therefore, it is necessary to provide a kind of production method that can make tone in green zircon-vanadium blue pigment blue.
Summary of the invention
It is an object of the invention to overcome drawbacks described above, a kind of Vanadium zirconium blue that the tone for making Vanadium zirconium blue is blue in blueness is provided The production method of colorant.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention are as follows:
A kind of production method of zircon-vanadium blue pigment, comprising the following steps:
Step 1 is mixed fluxing agent, binder and the first toner by following parts by weight: 20-25 parts of fluxing agent, bonding 5-10 parts of agent, the first 65-75 parts of toner, granulation is handled after mixing, obtains the second toner;
Step 2, by resulting second toner of zircon sand and step 1 at 2500-3000 DEG C cooling treatment after melting, and It is dried at 100-200 DEG C, obtains electric-melting zirconia;
Step 3 grinds the resulting electric-melting zirconia of step 2, control the granularity of electric-melting zirconia 13-18 μm it Between;
Step 4, the colorant of vanadium zirconium and auxiliary material are mixed and are ground with the resulting electric-melting zirconia of step 3, after grinding It at the uniform velocity heats up 8-10 hours to 750-850 DEG C, keeps the temperature 2 hours later, taken out after cooling down, obtain zircon-vanadium blue pigment.
Further, in the step 1, granulation processing is carried out with pelletizer, granule size controls 1-2mm.
Further, in the step 2, spectral measurement is carried out to obtained electric-melting zirconia, when adjusting in electric-melting zirconia When the mass fraction of toner is less than 0.3%, continue the operation of step 2, until the quality of toner is divided in electric-melting zirconia Number is 0.3%-0.8%.
Further, the mass fraction of toner is 0.3%-0.5% in the electric-melting zirconia that the step 2 obtains.
Further, in the step 3, granularity control is ground by ball-grinding machine, and is observed by laser particle analyzer Control.
Further, in the step 4, the mass fraction for obtaining electric-melting zirconia in zircon-vanadium blue pigment is 50%-60%.
Further, the holding temperature in the step 4 is 800 DEG C.
The beneficial effects of the present invention are: by zircon sand and toner high melt, electric-melting zirconia is obtained, controls electric smelting The content of toner in zirconium oxide, and control the granularity of electric-melting zirconia, to meet the color development demand of tone, finally plus Vanadium zirconium blue Colorant and other auxiliary materials be made zircon-vanadium blue pigment;The zircon-vanadium blue pigment produced changes original in green tune blue Electric-melting zirconia makes the dark tone blue of zircon-vanadium blue pigment, meets domestic ceramics and art ceramics industry to green tune blue Demand enriches the color of ceramic.
Detailed description of the invention
Fig. 1 is the process flow chart of the production method of zircon-vanadium blue pigment of the embodiment of the present invention.
Specific embodiment
In order to describe the technical content, the structural feature, the achieved object and the effect of this invention in detail, below in conjunction with embodiment And attached drawing is cooperated to be explained in detail.
The most critical design of the present invention is: toner and zircon sand high melt obtain electric-melting zirconia, electric smelting is controlled The content of the second toner is produced so that the hair color effect of electric-melting zirconia is good in the granularity and electric-melting zirconia of zirconium oxide Zircon-vanadium blue pigment in green tune blue.
Referring to Fig. 1, the production method of the zircon-vanadium blue pigment of the present embodiment, comprising the following steps:
Step 1 is mixed fluxing agent, binder and the first toner by following parts by weight: 20-25 parts of fluxing agent, bonding 5-10 parts of agent, the first 65-75 parts of toner carries out granulation processing after mixing completely in pelletizer, obtains the second toner, complete At the production of toner;
Step 2, by resulting second toner of zircon sand and step 1 at 2500-3000 DEG C after melting with industry water into Row cooling treatment, and dried at 100-200 DEG C, obtain electric-melting zirconia, i.e., after high melt processing and drying and processing To electric-melting zirconia;
Step 3 grinds the resulting electric-melting zirconia of step 2, control the granularity of electric-melting zirconia 13-18 μm it Between, and granularity is detected, if meeting granularity requirements carries out subsequent operation, not up to granularity requirements need to continue at grinding Reason;
Obtained by step 4, the colorant (vanadic anhydride) of vanadium zirconium and auxiliary material (Nacl, silica flour etc.) and step 3 Electric-melting zirconia mix and grind, at the uniform velocity heat up after grinding 8-10 hours to 750-850 DEG C, later keep the temperature 2 hours, cooling It is taken out after cooling, obtains zircon-vanadium blue pigment, complete the preparation of sample.
As can be seen from the above description, the beneficial effects of the present invention are: after zircon sand and toner high melt, obtain electricity Molten zirconium oxide, controls the content of toner and the granularity of electric-melting zirconia in electric-melting zirconia, to meet the color development demand of tone, Finally plus the obtained zircon-vanadium blue pigment such as other raw materials such as vanadic anhydride, Nacl of Vanadium zirconium blue;The zircon-vanadium blue pigment produced In green tune blue, the dark tone blue of original electric-melting zirconia production zircon-vanadium blue pigment is changed, domestic ceramics and work are met Demand of the skill ceramic industry to green tune blue, enriches the color of ceramic;
Further, in the step 1, granulation processing is carried out with pelletizer, granule size controls 1-2mm.
Seen from the above description, the granularity control of toner is 1-2mm, and toner can be made sufficiently to fuse with zircon sand.
Further, in the step 2, spectral measurement is carried out to obtained electric-melting zirconia, when adjusting in electric-melting zirconia When the mass fraction of toner is less than 0.3%, continue the operation of step 2, until the quality of toner is divided in electric-melting zirconia Number is 0.3%-0.8%.
Further, the mass fraction of toner is 0.3%-0.5% in the electric-melting zirconia that the step 2 obtains.
Seen from the above description, spectral measurement mainly detect electric-melting zirconia in zirconium oxide, silica, aluminium oxide, The content of titanium oxide, so that it is determined that the chemical composition content of electric-melting zirconia, then obtains toner in electric-melting zirconia;It adjusts Toner content controls the mainly adjustment to green tune blue, and the mass fraction of toner is 0.3%-0.5% in electric-melting zirconia When, it is in preferable hair color effect.
Further, in the step 3, granularity control is ground by ball-grinding machine, and is observed by laser particle analyzer Control.
Seen from the above description, laser particle analyzer can accurately control the grind size of electric-melting zirconia.
Further, in the step 4, the mass fraction for obtaining electric-melting zirconia in zircon-vanadium blue pigment is 50%-60%.
Seen from the above description, the content of electric-melting zirconia is 50%-60% in zircon-vanadium blue pigment, so that electric-melting zirconia Proportion between other raw materials of Vanadium zirconium blue is best, and Vanadium zirconium blue obtained meets color development requirement.
Further, the holding temperature in the step 4 is 800 DEG C.
Seen from the above description, 800 DEG C are the preferable reaction temperature of zircon-vanadium blue pigment, may make preparation process material reaction Completely.
It please refers to shown in Fig. 1, the embodiment of the present invention one are as follows:
A kind of production method of zircon-vanadium blue pigment, comprising the following steps:
Step 1 is mixed fluxing agent, binder and the first toner by following parts by weight: 25 parts of fluxing agent (sodium fluoride), 5 parts of binder (sodium metasilicate), 70 parts of toner (lithium carbonate) are carried out at granulation in pelletizer after mixing by blender Reason is granulated size controlling in 1mm, obtains the second toner;
Step 2 after melting, carries out resulting second toner of zircon sand and step 1 cold at 2750 DEG C with industry water But it handles, and dries be dried for standby under conditions of DEG C temperature at 150, high melt treated electric-melting zirconia carries out spectrum Measurement then continues to the processing of electric-melting zirconia high melt, directly when the content of toner in electric-melting zirconia is less than 0.3% Into the electric-melting zirconia of addition, the content 0.4% of toner, obtains electric-melting zirconia;
The resulting electric-melting zirconia of step 2 is ground by ball-grinding machine, and is carried out by laser particle analyzer by step 3 Observation control, the granularity for controlling electric-melting zirconia is 15 μm;
Step 4, the colorant (vanadic anhydride) of vanadium zirconium and auxiliary material (Nacl, silica flour, sodium fluoride) and step 3 Resulting electric-melting zirconia is mixed and is ground, and the effect of auxiliary material is to synthesize zircon-vanadium blue pigment at a lower temperature, after grinding It at the uniform velocity heats up in calcining furnace 9 hours to 800 DEG C, keeps the temperature 2 hours at a temperature of 800 DEG C later, take out, obtain after cooling down To zircon-vanadium blue pigment, the mass fraction of electric-melting zirconia is 60% in zircon-vanadium blue pigment.
The embodiment of the present invention two are as follows:
A kind of production method of zircon-vanadium blue pigment, comprising the following steps:
Step 1 is mixed fluxing agent, binder and the first toner by following parts by weight: 20 parts of fluxing agent (potassium chloride), 5 parts of binder (sodium metasilicate), 75 parts of toner (sodium carbonate) are carried out at granulation in pelletizer after mixing by blender Reason is granulated size controlling in 2mm, obtains the second toner;
Step 2 cools down resulting second toner of zircon sand and step 1 at 2500 DEG C with industry water after melting Processing, is then dried for standby under conditions of 100 DEG C of temperature, and high melt treated electric-melting zirconia carries out spectral measurement, When the content of toner in electric-melting zirconia is less than 0.3%, then continue to the processing of electric-melting zirconia high melt, until being added Electric-melting zirconia in toner content 0.5%, obtain electric-melting zirconia;
The resulting electric-melting zirconia of step 2 is ground by ball-grinding machine, and is carried out by laser particle analyzer by step 3 Observation control, the granularity for controlling electric-melting zirconia is 13 μm;
Step 4, the colorant (vanadic anhydride) of vanadium zirconium and auxiliary material (Nacl, silica flour, sodium fluoride) and step 3 Resulting electric-melting zirconia is mixed and is ground, and the effect of auxiliary material is to synthesize zircon-vanadium blue pigment at a lower temperature, after grinding It at the uniform velocity heats up in calcining furnace 10 hours to 850 DEG C, keeps the temperature 2 hours at a temperature of 800 DEG C later, taken out after cooling down, Zircon-vanadium blue pigment is obtained, the mass fraction of electric-melting zirconia is 50% in zircon-vanadium blue pigment.
Color development inspection is that the confirmation of the quality of the invention effect embodies, and the zircon-vanadium blue pigment made is ground into 350 mesh Powder product, be added in ceramic glaze in 5% mass fraction ratio, then Low fire ceramic at a temperature of 1250 DEG C, after cooling Hair color effect is examined with color difference meter.
Treated zircon-vanadium blue pigment is tested by color development, and experimental result is as shown in table 1,
1 zircon-vanadium blue pigment color development value of chromatism contrast table of table
The hair of the zircon-vanadium blue pigment produced by the electric-melting zirconia of addition toner is shown from the color development experimental result of table 1 The generation of color tone is more substantially change, and color development quality is better than the effect of standard sample, and color development tone is suitble to domestic ceramics and technique Ceramic effects of demand.
In conclusion the production method of zircon-vanadium blue pigment provided by the invention, prepares the partial size of regulator time control manufacture grain, Toner and zircon sand obtained is set sufficiently to fuse in high melt;The content of toner in zirconium oxide after controlling melting And the adjustment of toner content is carried out by spectral measurement;It mixes colours in granularity and electric-melting zirconia by controlling electric-melting zirconia The content of agent makes the Vanadium zirconium blue produced be in preferable hair color effect, finally plus other raw materials of Vanadium zirconium blue and controls correlation Reaction temperature produce zircon-vanadium blue pigment, the zircon-vanadium blue pigment produced changes original electric-melting zirconia in green tune blue Make the dark tone blue of zircon-vanadium blue pigment;Add the color development tone hair of the zircon-vanadium blue pigment of the electric-melting zirconia production of toner Life is more substantially change, and color development quality is better than the effect of standard sample, meets domestic ceramics and art ceramics industry to green blue The demand of tone enriches the color of ceramic.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair Equivalent structure or equivalent flow shift made by bright specification and accompanying drawing content is applied directly or indirectly in other relevant skills Art field, is included within the scope of the present invention.

Claims (5)

1. a kind of production method of the zircon-vanadium blue pigment in green tune blue, which comprises the steps of:
Step 1 is mixed fluxing agent, binder and the first toner by following parts by weight: 20 parts of fluxing agent, 5 parts of binder, the One 75 parts of toner, granulation is handled after mixing, obtains the second toner;
The fluxing agent is potassium chloride, and the binder is sodium metasilicate, and first toner is sodium carbonate;
Step 2, by resulting second toner of zircon sand and step 1 at 2500-3000 DEG C cooling treatment after melting, and It is dried at 100-200 DEG C, obtains electric-melting zirconia;
The mass fraction of the second toner is 0.5% in the electric-melting zirconia;
Step 3 grinds the resulting electric-melting zirconia of step 2, controls the granularity of electric-melting zirconia between 13 μm;
Step 4, the colorant of vanadium zirconium and auxiliary material are mixed and are ground with the resulting electric-melting zirconia of step 3, after grinding at the uniform velocity 8-10 hours to 750-850 DEG C of heating keeps the temperature 2 hours later, takes out after cooling down, obtains zircon-vanadium blue pigment;Described Toner is vanadic anhydride, and the auxiliary material is the mixture of Nacl, silica flour and sodium fluoride.
2. the production method of the zircon-vanadium blue pigment according to claim 1 in green tune blue, it is characterised in that: the step In 1, granulation processing is carried out with pelletizer, granule size controls 1-2mm.
3. the production method of the zircon-vanadium blue pigment according to claim 1 in green tune blue, it is characterised in that: the step In 3, granularity control is ground by ball-grinding machine, and carries out observation control by laser particle analyzer.
4. the production method of the zircon-vanadium blue pigment according to claim 1 in green tune blue, it is characterised in that: the step In 4, the mass fraction for obtaining electric-melting zirconia in zircon-vanadium blue pigment is 50%-60%.
5. the production method of the zircon-vanadium blue pigment according to claim 1 in green tune blue, it is characterised in that: the step Holding temperature in 4 is 800 DEG C.
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CN113248254A (en) * 2021-06-08 2021-08-13 三祥新材股份有限公司 Method for improving temperature resistance of vanadium-zirconium blue pigment produced by electrically-fused zirconia

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CN108250804B (en) * 2018-01-31 2020-05-05 洛阳师范学院 Nano vanadium-zirconium blue ceramic pigment and preparation method thereof
CN111849207B (en) * 2020-08-13 2021-09-10 三祥新材股份有限公司 Method for improving blue value of vanadium-zirconium blue pigment
CN113264673A (en) * 2021-06-08 2021-08-17 三祥新材股份有限公司 Method for producing yellowish-red zirconium-iron-red regulating pigment by electrically melting zirconia

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