CN108610658A - A kind of preparation method of zircon-vanadium blue pigment at low cost - Google Patents
A kind of preparation method of zircon-vanadium blue pigment at low cost Download PDFInfo
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- CN108610658A CN108610658A CN201810211037.7A CN201810211037A CN108610658A CN 108610658 A CN108610658 A CN 108610658A CN 201810211037 A CN201810211037 A CN 201810211037A CN 108610658 A CN108610658 A CN 108610658A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
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- 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
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of 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
- C09C3/003—Flushing
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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
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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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
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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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
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/043—Drying, calcination
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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
Abstract
The present invention relates to a kind of preprocess methods of zirconium English powder, it carries out zirconium English powder to be heated and pressurizeed processing, the temperature of the heat treatment is 350 400 DEG C, the pressure of the pressurized treatments is 0.4 0.6MPa, then being heated and pressurizeed that treated, zirconium English powder carries out pickling to neutrality, zirconium English powder after pickling is first dried and is ground again, pretreated zirconium English powder is obtained.The invention further relates to a kind of preparation methods of zircon-vanadium blue pigment.The preprocess method of the zirconium English powder of the present invention can substantially reduce reaction impurities and significantly improve the reactivity of zirconium English powder;The preparation method of the zircon-vanadium blue pigment of the present invention has the advantages that improve yield and method is simple and easy to control.
Description
This case is with the applying date on 01 26th, 2016, application No. is 201610051838.2, it is entitled " zirconium English powder
The divisional application that the patent of invention of the preparation method of preprocess method and zircon-vanadium blue pigment " carries out for female case.
Technical field
The present invention relates to colorant production technology, more particularly to the preprocess method of a kind of zirconium English powder and zircon-vanadium blue pigment
Preparation method.
Background technology
Ceramic pigment industry seldom produces zircon-vanadium blue pigment, mainly zirconium English powder knot using zirconium English powder as raw material at present
Structure is stablized, the reason of being firmly combined between key and key.But the requirement of electric smelting zirconium is not achieved in it in terms of composition and activity, simultaneously
The content of the impurity such as its aluminium oxide and titanium oxide is higher.Zirconium English powder need to be pre-processed, be allowed to meet the anti-of zircon-vanadium blue pigment
It should require.
The patent of invention of Patent No. 03131530.5 discloses a kind of vanadium zirconium indigo plant pigment manufacturing method, with zircon sand, pure
Alkali, vfanadium compound and halide are raw material, are made through ball milling, roast, ball milling, washing, drying, phosphate is added in raw material,
Hydrogen fluoride and sulfur trioxide gas are passed through when roasting.This method makes the raw material of manufacture vanadium zirconium indigo plant pigment reach more uniform ideal
Admixture, the tinctorial strength of the vanadium zirconium indigo plant pigment of manufacture and bright-colored degree are more preferable.But pretreated zirconium English powder
That there are still reactivities is low, impurity content is higher, and then deficiency of high cost;The vanadium zirconium indigo plant pigment prepared using the above method
The also Shortcomings in terms of composition purity and activity.
Invention content
The technical problem to be solved by the present invention is to:A kind of pre- place effectively improving purity and active zirconium English powder is provided
Reason method, and a kind of preparation method of zircon-vanadium blue pigment is provided on this basis.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is:
A kind of preprocess method of zirconium English powder carries out zirconium English powder to be heated and pressurizeed processing, the temperature of the heat treatment
It it is 350-400 DEG C, the pressure of the pressurized treatments is 0.4-0.6MPa, and being then heated and pressurizeed that treated, zirconium English powder carries out
Zirconium English powder after pickling is first dried and is ground again, obtain pretreated zirconium English powder to neutrality by pickling.
The present invention also provides a kind of preparation methods of zircon-vanadium blue pigment, and the preprocess method of above-mentioned zirconium English powder is pre-processed
Zirconium English powder, vanadic anhydride and sodium chloride mixing afterwards, obtain mixture, are then by the mixture constant-speed heating to temperature
800-900 DEG C, time of the heating is 8-11h, and mixture temperature is maintained to be 800-900 DEG C and continue 1-1.5h, then into
Row cooling, obtains zircon-vanadium blue pigment.
The beneficial effects of the present invention are:
(1) preprocess method of zirconium English powder of the invention, it is above-mentioned be heated and pressurizeed processing can effectively will be in zirconium English powder
Zirconium oxide and silica associative key are opened, and are realized fully de- key, are taken off key rate up to 98% or more;Pickling has removal of impurities effect,
Drying can further cure removal of impurities, can substantially reduce reaction impurities;Grinding can control the granularity of zirconium English powder, i.e.,
By taking off key, solidification except the technological design of impurity and granularity control, zirconium English powder is pre-processed, impurity effect is being substantially eliminated
In the case of, the reactivity of zirconium English powder can be significantly improved;
(2) preparation method of zircon-vanadium blue pigment of the invention, by pretreated zirconium English powder and vanadic anhydride, sodium chloride
Raw material progress Hybrid Heating is prepared Deng other vanadium zirconium indigo plants, above-mentioned mode of heating can improve the conversion ratio of zirconium English powder, have abundant
Using raw material, improve yield and method advantage simple and easy to control;
(3) electric-melting zirconia production zircon-vanadium blue pigment can be substituted, the production cost of zircon-vanadium blue pigment is reduced.
Specific implementation mode
To explain the technical content, the achieved purpose and the effect of the present invention in detail, it is explained below in conjunction with embodiment.
The design of most critical of the present invention is:By the technological design for taking off key, solidification removes impurity and granularity controls, to zirconium English
Powder is pre-processed, to significantly improve reactivity.
The present invention provides a kind of preprocess method of zirconium English powder, and zirconium English powder is carried out to be heated and pressurizeed processing, the heating
The temperature of processing is 350-400 DEG C, and the pressure of the pressurized treatments is 0.4-0.6MPa, then will be heated and pressurizeed that treated
Zirconium English powder carries out pickling to neutrality, and the zirconium English powder after pickling is first dried and is ground again, pretreated zirconium English is obtained
Powder.
The present invention also provides a kind of preparation methods of zircon-vanadium blue pigment, and the preprocess method of above-mentioned zirconium English powder is pre-processed
Zirconium English powder, vanadic anhydride and sodium chloride mixing afterwards, obtain mixture, are then by the mixture constant-speed heating to temperature
800-900 DEG C, time of the heating is 8-11h, and mixture temperature is maintained to be 800-900 DEG C and continue 1-1.5h, then into
Row cooling, obtains zircon-vanadium blue pigment.
As can be seen from the above description, the beneficial effects of the present invention are:
(1) preprocess method of zirconium English powder of the invention, it is above-mentioned be heated and pressurizeed processing can effectively will be in zirconium English powder
Zirconium oxide and silica associative key are opened, and are realized fully de- key, are taken off key rate up to 98% or more;Pickling has removal of impurities effect,
Drying can further cure removal of impurities, can substantially reduce reaction impurities;Grinding can control the granularity of zirconium English powder, i.e.,
By taking off key, solidification except the technological design of impurity and granularity control, zirconium English powder is pre-processed, impurity effect is being substantially eliminated
In the case of, the reactivity of zirconium English powder can be significantly improved;
(2) preparation method of zircon-vanadium blue pigment of the invention, by pretreated zirconium English powder and vanadic anhydride, sodium chloride
Raw material progress Hybrid Heating is prepared Deng other vanadium zirconium indigo plants, above-mentioned mode of heating can improve the conversion ratio of zirconium English powder, have abundant
Using raw material, improve yield and method advantage simple and easy to control;
(3) electric-melting zirconia production zircon-vanadium blue pigment can be substituted, the production cost of zircon-vanadium blue pigment is reduced.
In the preprocess method of the zirconium English powder of the present invention:
Further, the pickling uses mass concentration for the sulfuric acid of 1-2% or hydrochloric acid.By zirconium English powder pickling to impurity matter
It measures concentration and is less than 0.1%, the impurity includes Al2O3、Fe2O3、TiO2And P2O5At least one of.
Seen from the above description, the sulfuric acid or hydrochloric acid that mass concentration is 1-2% can be used in pickling;It can be to the zirconium after pickling
English powder carries out spectral measurement, when impurity content is more than 0.1%, continues to carry out pickling to zirconium English powder, until impurity mass concentration is equal
Less than 0.1%, preferred impurity mass concentration can be less than 0.06%.
Further, described to be ground to the granularity control of zirconium English powder be 5-10 μm.
Seen from the above description, granularity control can be ground by ball-grinding machine, and carry out observation control by laser particle analyzer
System.Preferably, granularity control is 5-10 μm, can further increase the surface area of zirconium English powder, keep reaction more abundant.
In the preparation method of the zircon-vanadium blue pigment of the present invention:
Further, first the mixture is ground, then carries out constant-speed heating.
Seen from the above description, first mixture can be ground before constant-speed heating, is ground to as needed certain
Granularity, further promote reaction progress, can be improved reaction efficiency, shorten the reaction time.
The embodiment of the present invention one is:
A kind of preparation method of zircon-vanadium blue pigment of the present embodiment carries out zirconium English powder to be heated and pressurizeed processing, described to add
The temperature of heat treatment is 350 DEG C, and the pressure of the pressurized treatments is 0.4MPa, the zirconium English powder that then will be heated and pressurizeed that treated
It uses mass concentration to carry out pickling for 1% sulfuric acid or hydrochloric acid and controls Al to neutrality, while by pickling2O3、Fe2O3、TiO2With
P2O5Impurity mass concentration is 0.1%.Zirconium English powder after pickling is first dried and is ground again with by the granularity control of zirconium English powder
5 μm are made as, pretreated zirconium English powder is obtained.
The pretreated zirconium English powder of preprocess method, vanadic anhydride and the sodium chloride of above-mentioned zirconium English powder (can also be added
Enter other zircon-vanadium blue pigments in the prior art prepares raw material) uniformly mixing, mixture is obtained, first grinds the mixture
Then the mixture constant-speed heating to temperature is 800 DEG C by mill, the time of the heating is 8h, and maintenance mixture temperature is
800 DEG C and continue 1h, then cooled down, obtains zircon-vanadium blue pigment.
The embodiment of the present invention two is:
A kind of preparation method of zircon-vanadium blue pigment of the present embodiment carries out zirconium English powder to be heated and pressurizeed processing, described to add
The temperature of heat treatment is 400 DEG C, and the pressure of the pressurized treatments is 0.6MPa, the zirconium English powder that then will be heated and pressurizeed that treated
It uses mass concentration to carry out pickling for 2% sulfuric acid or hydrochloric acid and controls Al to neutrality, while by pickling2O3、Fe2O3、TiO2With
P2O5Impurity mass concentration is 0.01%.Zirconium English powder after pickling is first dried and is ground again with by the granularity of zirconium English powder
Control is 10 μm, obtains pretreated zirconium English powder.
The pretreated zirconium English powder of preprocess method, vanadic anhydride and the sodium chloride of above-mentioned zirconium English powder (can also be added
Enter other zircon-vanadium blue pigments in the prior art prepares raw material) uniformly mixing, mixture is obtained, first grinds the mixture
Then the mixture constant-speed heating to temperature is 900 DEG C by mill, the time of the heating is 11h, and maintenance mixture temperature is
900 DEG C and continue 1.5h, then cooled down, obtains zircon-vanadium blue pigment.
The embodiment of the present invention three is:
A kind of preparation method of zircon-vanadium blue pigment of the present embodiment carries out zirconium English powder to be heated and pressurizeed processing, described to add
The temperature of heat treatment is 380 DEG C, and the pressure of the pressurized treatments is 0.5MPa, the zirconium English powder that then will be heated and pressurizeed that treated
It uses mass concentration to carry out pickling for 1.5% sulfuric acid or hydrochloric acid and controls Al to neutrality, while by pickling2O3、Fe2O3、TiO2
And P2O5Impurity mass concentration is 0.05%.Zirconium English powder after pickling is first dried and is ground again with by the grain of zirconium English powder
Degree control is 8 μm, obtains pretreated zirconium English powder.
The pretreated zirconium English powder of preprocess method, vanadic anhydride and the sodium chloride of above-mentioned zirconium English powder (can also be added
Enter other zircon-vanadium blue pigments in the prior art prepares raw material) uniformly mixing, mixture is obtained, first grinds the mixture
Then the mixture constant-speed heating to temperature is 850 DEG C by mill, the time of the heating is 10h, and maintenance mixture temperature is
850 DEG C and continue 1.2h, then cooled down, obtains zircon-vanadium blue pigment.
The embodiment of the present invention four is:
A kind of preparation method of the zircon-vanadium blue pigment of the present embodiment,
Include the following steps:
1):De- key processing:By common zirconium English powder, is handled under certain temperature and pressure by reaction kettle, make zirconium English
Zirconium oxide and silica associative key opening meet zircon-vanadium blue pigment reaction requirement in powder;
2) solidification removes impurity:Step 1) products therefrom is washed with diluted acid, the diluted acid can be that 2% (quality) is dilute
Sulfuric acid or dilute hydrochloric acid, impurity A l in pickling to zirconium English powder2O3、Fe2O3、TiO2、P2O5Content is respectively less than 0.1% (quality), process
In take sample segment by spectral detection such as ray fluorescence spectrometer, if Al2O3、Fe2O3、TiO2、P2O5Content is more than 0.1%
When (quality), continue to carry out pickling to zirconium English powder, until Al2O3、Fe2O3、TiO2、P2O5It, will after content is less than 0.1% (quality)
The zirconium English powder of removal of impurities is dried;
3) granularity controls:It removes the zirconium English powder after impurity to step 2) to be ground, process is carried out using vertical mixer
Grinding, and observed by Malvern ParticleSizer, the granularity of zirconium English powder is controlled between 5-10 μm;
4) sample is prepared:The zirconium English powder and other raw materials of vanadium zirconium blue obtained by step 3) are weighed, is sufficiently mixed according to formula, mistake
In journey using dry bulb mill carry out mixed grinding, it is levigate after in cabinet-type electric furnace or high temperature furnace 10 hours of heating and calcining, temperature set
It is set to 800-900 DEG C, 1 hour is kept the temperature after reaching preset temperature, is taken out after cooling.
Measure of merit
Zircon-vanadium blue pigment that embodiment one to example IV is prepared and in the prior art electric-melting zirconia method
The zircon-vanadium blue pigment of acquisition carries out color development experiment respectively, and color development experimental result is as shown in table 1.Table 1 be the embodiment of the present invention one to
The color development for the zircon-vanadium blue pigment that the electric-melting zirconia method for the zircon-vanadium blue pigment and the prior art that example IV prepares obtains
Experimental result contrast table.
Table 1
As shown in Table 1, the zircon-vanadium blue pigment that the embodiment of the present invention one is obtained to example IV, which all has, meets or exceeds electricity
The hair color effect of molten zirconium oxide, zircon-vanadium blue pigment prepared by the nearly electric-melting zirconia of illuminant colour differential.
Specifically, the Al in zirconium English powder can be effectively reduced2O3、Fe2O3、TiO2、P2O5Content, reduce reaction impurities
Influence, and control the granularity of zirconium English powder, improve its reactivity, be more advantageous to the production of zircon-vanadium blue pigment, can be complete
Replace electric-melting zirconia, reduces the production cost of zircon-vanadium blue pigment.
Curing deimpurity process, it generally can be by Al2O3、Fe2O3、TiO2、P2O5Content be down to respectively be 0.06%
(quality) can ignore the influence of impurity in the production that zirconium English powder prepares zircon-vanadium blue pigment, reach ideal effect at this time.
The best holding temperature is 850 DEG C, keeps the temperature 1 hour at such a temperature so that preparation process material reaction
Completely.
In conclusion the preprocess method of zirconium English powder provided by the invention can substantially reduce reaction impurities and significantly improve
The reactivity of zirconium English powder;The preparation method of the zircon-vanadium blue pigment of the present invention, which has, improves yield and simple and easy to control excellent of method
Point.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair
Equivalents made by bright description are applied directly or indirectly in relevant technical field, are similarly included in this hair
In bright scope of patent protection.
Claims (2)
1. a kind of preparation method of zircon-vanadium blue pigment at low cost, which is characterized in that
Zirconium English powder is carried out to be heated and pressurizeed processing, the temperature of the heat treatment is 350-400 DEG C, the pressure of the pressurized treatments
Power is 0.4-0.6MPa, and being then heated and pressurizeed that treated, zirconium English powder carries out pickling to neutrality, by the zirconium English powder after pickling
It is first dried and is ground again, obtain pretreated zirconium English powder;It is described to be ground to the granularity control of zirconium English powder be 5-10 μ
m;The pickling uses mass concentration for the sulfuric acid of 1-2% or hydrochloric acid;Zirconium English powder pickling to impurity mass concentration is less than
0.1%, the impurity includes Al2O3、Fe2O3、TiO2And P2O5At least one of;
The pretreated zirconium English powder, vanadic anhydride and sodium chloride of acquisition are mixed, mixture is obtained, then by the mixing
Object constant-speed heating to temperature is 800-900 DEG C, and time of the heating is 8-11h, maintain mixture temperature be 800-900 DEG C simultaneously
Continue 1-1.5h, then cooled down, obtains zircon-vanadium blue pigment.
2. the preparation method of zircon-vanadium blue pigment at low cost according to claim 1, which is characterized in that first by the mixing
Object is ground, then carries out constant-speed heating.
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CN107118589B (en) * | 2017-05-08 | 2018-11-13 | 三祥新材股份有限公司 | A kind of production method of zircon-vanadium blue pigment |
CN112694326A (en) * | 2020-12-30 | 2021-04-23 | 泉州市利芝新材料科技有限公司 | Zircon sand iron removal process |
CN112723366A (en) * | 2020-12-30 | 2021-04-30 | 泉州市利芝新材料科技有限公司 | Process for removing iron and titanium from zircon sand |
CN115141016A (en) * | 2022-07-28 | 2022-10-04 | 宜兴市海科耐火材料制品有限公司 | Preparation method of high-reactivity combined zircon powder special for precision casting |
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CN105733310A (en) | 2016-07-06 |
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