CN105733310A - Pretreatment method of zircon powder and preparation method of vanadium-zirconium blue material - Google Patents
Pretreatment method of zircon powder and preparation method of vanadium-zirconium blue material Download PDFInfo
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- CN105733310A CN105733310A CN201610051838.2A CN201610051838A CN105733310A CN 105733310 A CN105733310 A CN 105733310A CN 201610051838 A CN201610051838 A CN 201610051838A CN 105733310 A CN105733310 A CN 105733310A
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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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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
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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
- 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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- 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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- 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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- 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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- 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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Abstract
The invention relates to a pretreatment method of zircon powder. The pretreatment method comprises: performing heating and pressurizing treatments on zircon powder, wherein the temperature of the heating treatment is 350-400 DEG C, and the pressure of the pressurizing treatment is 0.4-0.6MPa; then performing acid cleaning on the zircon powder after the heating and pressurizing treatments until the zircon powder is neutral; and performing drying at first and then performing grinding on the zircon powder after acid cleaning to obtain zircon powder after pretreatment. The invention also relates to a preparation method of a vanadium-zirconium blue material. The pretreatment method of the zircon powder, provided by the invention, can significantly reduce reaction impurities and significantly improve the reactivity of the zircon powder; and the preparation method of the vanadium-zirconium blue material, provided by the invention, has the advantages of improving the productive rate and being simple and easy to control.
Description
Technical field
The present invention relates to colorant production technology, preprocess method and vanadium zirconium particularly to a kind of zirconium English powder are blue
The preparation method of colorant.
Background technology
Ceramic pigment industry seldom uses zirconium English powder as raw material to produce zircon-vanadium blue pigment at present, mainly zirconium
English powder Stability Analysis of Structures, the reason being firmly combined with between key and key.But it does not reaches in terms of composition and activity
The requirement of electric smelting zirconium, the content of its impurity such as aluminium oxide and titanium oxide is higher simultaneously.Need to zirconium English powder be carried out pre-
Process, be allowed to meet the reaction requirement of zircon-vanadium blue pigment.
The patent of invention of Patent No. 03131530.5 discloses a kind of vanadium zirconium indigo plant pigment manufacture method, with zirconium English
Sand, soda, vfanadium compound and halogenide are raw material, through ball milling, roast, ball milling, wash, dry prepared,
Raw material is added with phosphate, during roasting, is passed through fluohydric acid gas and sulfur trioxide gas.The method makes manufacture vanadium zirconium
The raw material of blue pigment reaches the most even preferable admixture, the tinctorial strength of the vanadium zirconium indigo plant pigment of manufacture
More preferable with bright-colored degree.But, its pretreated zirconium English powder still suffers from that reactivity is low, impurity content
Higher, and then the deficiency that cost is high；Use the vanadium zirconium indigo plant pigment that said method is prepared in composition purity and work
Property aspect also Shortcomings.
Summary of the invention
The technical problem to be solved is: provide a kind of zirconium English powder being effectively improved purity and activity
Preprocess method, and provide the preparation method of a kind of zircon-vanadium blue pigment on this basis.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is:
The preprocess method of a kind of zirconium English powder, carries out heating and pressurized treatments by zirconium English powder, described heat treated
Temperature be 350-400 DEG C, the pressure of described pressurized treatments is 0.4-0.6MPa, then will heating and pressurization at
It is the most neutral that zirconium English powder after reason carries out pickling, first carries out drying being ground by the zirconium English powder after pickling again, obtains
Obtain pretreated zirconium English powder.
The present invention also provides for the preparation method of a kind of zircon-vanadium blue pigment, by the preprocess method of above-mentioned zirconium English powder
Pretreated zirconium English powder, vanadic anhydride and sodium chloride mixing, it is thus achieved that mixture, then by described mixing
Thing constant-speed heating to temperature is 800 900 DEG C, and the time of described heating is 8 11h, and maintenance mixture temperature is
800 900 DEG C and lasting 1 1.5h, then cool down, it is thus achieved that zircon-vanadium blue pigment.
The beneficial effects of the present invention is:
(1) preprocess method of the zirconium English powder of the present invention, above-mentioned heating and pressurized treatments can be effectively by zirconiums
In English powder, zirconium oxide and silicon dioxide associative key are opened, it is achieved fully take off key, and de-key rate is up to more than 98%；
Pickling has remove impurity effect, and drying can solidify remove impurity further, can substantially reduce reaction impurities；Grind
The granularity of zirconium English powder can be controlled, i.e. be set by the technique of de-key, the solidification removal of impurity and Task-size Controlling
Meter, carries out pretreatment to zirconium English powder, in the case of substantially eliminating impurity effect, can significantly improve zirconium English
The reactivity of powder；
(2) preparation method of the zircon-vanadium blue pigment of the present invention, by pretreated zirconium English powder and vanadic anhydride,
Other vanadium zirconium indigo plants such as sodium chloride are prepared raw material and are carried out Hybrid Heating, and above-mentioned mode of heating can improve zirconium English powder
Conversion ratio, has and makes full use of the advantage that raw material, raising productivity and method are simple and easy to control；
(3) can substitute electric-melting zirconia and produce zircon-vanadium blue pigment, the production decreasing zircon-vanadium blue pigment becomes
This.
Detailed description of the invention
By describing the technology contents of the present invention in detail, being realized purpose and effect, give below in conjunction with embodiment
With explanation.
The design of most critical of the present invention is: by de-key, the solidification removal of impurity and the technological design of Task-size Controlling,
Zirconium English powder is carried out pretreatment, thus significantly improves reactivity.
The present invention provides the preprocess method of a kind of zirconium English powder, carries out heating and pressurized treatments by zirconium English powder, institute
The temperature stating heat treated is 350-400 DEG C, and the pressure of described pressurized treatments is 0.4-0.6MPa, then will add
It is the most neutral that zirconium English powder after heat and pressurized treatments carries out pickling, first carries out drying entering by the zirconium English powder after pickling again
Row grinds, it is thus achieved that pretreated zirconium English powder.
The present invention also provides for the preparation method of a kind of zircon-vanadium blue pigment, by the preprocess method of above-mentioned zirconium English powder
Pretreated zirconium English powder, vanadic anhydride and sodium chloride mixing, it is thus achieved that mixture, then by described mixing
Thing constant-speed heating to temperature is 800 900 DEG C, and the time of described heating is 8 11h, and maintenance mixture temperature is
800 900 DEG C and lasting 1 1.5h, then cool down, it is thus achieved that zircon-vanadium blue pigment.
Knowable to foregoing description, the beneficial effects of the present invention is:
(1) preprocess method of the zirconium English powder of the present invention, above-mentioned heating and pressurized treatments can be effectively by zirconiums
In English powder, zirconium oxide and silicon dioxide associative key are opened, it is achieved fully take off key, and de-key rate is up to more than 98%；
Pickling has remove impurity effect, and drying can solidify remove impurity further, can substantially reduce reaction impurities；Grind
The granularity of zirconium English powder can be controlled, i.e. be set by the technique of de-key, the solidification removal of impurity and Task-size Controlling
Meter, carries out pretreatment to zirconium English powder, in the case of substantially eliminating impurity effect, can significantly improve zirconium English
The reactivity of powder；
(2) preparation method of the zircon-vanadium blue pigment of the present invention, by pretreated zirconium English powder and vanadic anhydride,
Other vanadium zirconium indigo plants such as sodium chloride are prepared raw material and are carried out Hybrid Heating, and above-mentioned mode of heating can improve zirconium English powder
Conversion ratio, has and makes full use of the advantage that raw material, raising productivity and method are simple and easy to control；
(3) can substitute electric-melting zirconia and produce zircon-vanadium blue pigment, the production decreasing zircon-vanadium blue pigment becomes
This.
In the preprocess method of the zirconium English powder of the present invention:
Further, sulphuric acid or the hydrochloric acid that described pickling uses mass concentration to be 1-2%.By zirconium English powder pickling extremely
Impurity mass concentration is less than 0.1%, and described impurity includes Al2O3、Fe2O3、TiO2And P2O5In at least one
Kind.
Seen from the above description, pickling can use mass concentration to be 1-2% sulphuric acid or hydrochloric acid；Can be to pickling
After zirconium English powder carry out spectral measurement, impurity content more than 0.1% time, continue zirconium English powder is carried out pickling, directly
Being respectively less than 0.1% to impurity mass concentration, preferred impurity mass concentration can be less than 0.06%.
Further, being ground to the Task-size Controlling of zirconium English powder described in is 5-10 μm.
Seen from the above description, Task-size Controlling can be ground by ball-grinding machine, and is carried out by laser particle analyzer
Observe and control.Preferably, Task-size Controlling is 5-10 μm, can improve the surface area of zirconium English powder further, make
React more abundant.
In the preparation method of the zircon-vanadium blue pigment of the present invention:
Further, first described mixture is ground, then carry out constant-speed heating.
Seen from the above description, first mixture can be ground before constant-speed heating, grind as required
To certain granularity, promote the carrying out of reaction further, reaction efficiency can be improved, shorten the response time.
Embodiments of the invention one are:
The preparation method of a kind of zircon-vanadium blue pigment of the present embodiment, carries out heating and pressurized treatments by zirconium English powder,
The temperature of described heat treated is 350 DEG C, and the pressure of described pressurized treatments is 0.4MPa, then will heating and
Sulphuric acid or hydrochloric acid that zirconium English powder after pressurized treatments uses mass concentration to be 1% carry out pickling extremely neutrality, lead to simultaneously
Overpickling controls Al2O3、Fe2O3、TiO2And P2O5Impurity mass concentration is 0.1%.By the zirconium English after pickling
Powder first carries out drying and is ground with the Task-size Controlling by zirconium English powder being 5 μm again, it is thus achieved that pretreated zirconium English
Powder.
By preprocess method pretreated zirconium English powder, vanadic anhydride and the sodium chloride of above-mentioned zirconium English powder (also
Can add other zircon-vanadium blue pigment of the prior art prepares raw material) uniformly mix, it is thus achieved that mixture, first
Described mixture is ground, is then 800 DEG C by described mixture constant-speed heating to temperature, described heating time
Between be 8h, maintaining mixture temperature is 800 DEG C and lasting 1h, then cools down, it is thus achieved that zircon-vanadium blue pigment.
Embodiments of the invention two are:
The preparation method of a kind of zircon-vanadium blue pigment of the present embodiment, carries out heating and pressurized treatments by zirconium English powder,
The temperature of described heat treated is 400 DEG C, and the pressure of described pressurized treatments is 0.6MPa, then will heating and
Sulphuric acid or hydrochloric acid that zirconium English powder after pressurized treatments uses mass concentration to be 2% carry out pickling extremely neutrality, lead to simultaneously
Overpickling controls Al2O3、Fe2O3、TiO2And P2O5Impurity mass concentration is 0.01%.By the zirconium after pickling
English powder first carries out drying and is ground with the Task-size Controlling by zirconium English powder being 10 μm again, it is thus achieved that pretreated
Zirconium English powder.
By preprocess method pretreated zirconium English powder, vanadic anhydride and the sodium chloride of above-mentioned zirconium English powder (also
Can add other zircon-vanadium blue pigment of the prior art prepares raw material) uniformly mix, it is thus achieved that mixture, first
Described mixture is ground, is then 900 DEG C by described mixture constant-speed heating to temperature, described heating time
Between be 11h, maintaining mixture temperature is 900 DEG C and lasting 1.5h, then cools down, it is thus achieved that vanadium zirconium blueness
Material.
Embodiments of the invention three are:
The preparation method of a kind of zircon-vanadium blue pigment of the present embodiment, carries out heating and pressurized treatments by zirconium English powder,
The temperature of described heat treated is 380 DEG C, and the pressure of described pressurized treatments is 0.5MPa, then will heating and
Sulphuric acid or hydrochloric acid that zirconium English powder after pressurized treatments uses mass concentration to be 1.5% carry out pickling to neutral, simultaneously
Al is controlled by pickling2O3、Fe2O3、TiO2And P2O5Impurity mass concentration is 0.05%.After pickling
Zirconium English powder first carries out drying and is ground with the Task-size Controlling by zirconium English powder being 8 μm again, it is thus achieved that pretreated
Zirconium English powder.
By preprocess method pretreated zirconium English powder, vanadic anhydride and the sodium chloride of above-mentioned zirconium English powder (also
Can add other zircon-vanadium blue pigment of the prior art prepares raw material) uniformly mix, it is thus achieved that mixture, first
Described mixture is ground, is then 850 DEG C by described mixture constant-speed heating to temperature, described heating time
Between be 10h, maintaining mixture temperature is 850 DEG C and lasting 1.2h, then cools down, it is thus achieved that vanadium zirconium blueness
Material.
Embodiments of the invention four are:
A kind of preparation method of the zircon-vanadium blue pigment of the present embodiment,
Comprise the following steps:
1): de-key processes: by common zirconium English powder, processed under uniform temperature and pressure by reactor,
Make zirconium oxide and silicon dioxide associative key in zirconium English powder open and meet zircon-vanadium blue pigment reaction requirement；
2) the solidification removal of impurity: by step 1) products therefrom diluted acid washs, and described diluted acid can be 2%
(quality) dilute sulfuric acid or dilute hydrochloric acid, impurity A l in pickling to zirconium English powder2O3、Fe2O3、TiO2、P2O5Contain
Amount respectively less than 0.1% (quality), during take sample segment by spectral detection such as ray fluorescence spectrometer, as
Really Al2O3、Fe2O3、TiO2、P2O5When content is more than 0.1% (quality), continue zirconium English powder is carried out acid
Wash, until Al2O3、Fe2O3、TiO2、P2O5Content is less than after 0.1% (quality), by the zirconium English of remove impurity
Powder is dried；
3) Task-size Controlling: to step 2) go the removal of impurity after zirconium English powder be ground, process uses and vertical stirs
The machine of mixing is ground, and is observed by Malvern ParticleSizer, control zirconium English powder granularity 5-10 μm it
Between；
4) sample is prepared: weigh step 3) zirconium English powder and other raw materials of vanadium zirconium blue of gained, fill according to formula
Point mixing, during use dry bulb mill to carry out mixed grinding, levigate after heat in cabinet-type electric furnace or high temperature furnace
Calcining 10 hours, temperature is set to 800-900 DEG C, is incubated 1 hour, cooling after reaching preset temperature
Rear taking-up.
Measure of merit
Electric smelting oxidation in the zircon-vanadium blue pigment that embodiment one to embodiment four is prepared and prior art
The zircon-vanadium blue pigment that zirconium method obtains carries out color development experiment respectively, and color development experimental result is as shown in table 1.Table 1
The zircon-vanadium blue pigment prepared for the embodiment of the present invention one to embodiment four and the electric-melting zirconia of prior art
The color development experimental result contrast table of the zircon-vanadium blue pigment that method obtains.
Table 1
As shown in Table 1, the embodiment of the present invention one to embodiment four obtain zircon-vanadium blue pigment be respectively provided with reach or
Exceed the hair color effect of electric-melting zirconia, zircon-vanadium blue pigment prepared by its nearly electric-melting zirconia of illuminant color differential.
Concrete, the Al in zirconium English powder can be effectively reduced2O3、Fe2O3、TiO2、P2O5Content,
The impact of minimizing reaction impurities, and control the granularity of zirconium English powder, improve its reactivity, be more beneficial for vanadium
The production of zirconium blue, can replace electric-melting zirconia completely, reduces the production cost of zircon-vanadium blue pigment.
Solidifying deimpurity process, typically can be by Al2O3、Fe2O3、TiO2、P2O5Content be down to
It is respectively 0.06% (quality), now prepares the shadow that can ignore impurity in the production of zircon-vanadium blue pigment at zirconium English powder
Ring, reach preferable effect.
Described optimal holding temperature is 850 DEG C, at such a temperature insulation 1 hour so that preparation process thing
Material reaction is completely.
In sum, the preprocess method of the zirconium English powder that the present invention provides can substantially reduce reaction impurities and show
Write the reactivity improving zirconium English powder；The preparation method of the zircon-vanadium blue pigment of the present invention has raising productivity and side
The advantage that method is simple and easy to control.
The foregoing is only embodiments of the invention, not thereby limit the scope of the claims of the present invention, every profit
The equivalents made by description of the invention content, or directly or indirectly it is used in relevant technical field,
The most in like manner it is included in the scope of patent protection of the present invention.
Claims (6)
1. the preprocess method of a zirconium English powder, it is characterised in that carry out heating and pressurized treatments by zirconium English powder,
The temperature of described heat treated is 350-400 DEG C, and the pressure of described pressurized treatments is 0.4-0.6MPa, then will
It is the most neutral that zirconium English powder after heating and pressurized treatments carries out pickling, first carries out drying by the zirconium English powder after pickling again
It is ground, it is thus achieved that pretreated zirconium English powder.
The preprocess method of zirconium English powder the most according to claim 1, it is characterised in that described pickling is adopted
With the sulphuric acid that mass concentration is 1-2% or hydrochloric acid.
The preprocess method of zirconium English powder the most according to claim 1, it is characterised in that described in be ground to
It is 5-10 μm by the Task-size Controlling of zirconium English powder.
The preprocess method of zirconium English powder the most according to claim 1, it is characterised in that by the acid of zirconium English powder
Being washed till impurity mass concentration and be less than 0.1%, described impurity includes Al2O3、Fe2O3、TiO2And P2O5In extremely
Few one.
5. the preparation method of a zircon-vanadium blue pigment, it is characterised in that by claim 1-4 any one institute
The preprocess method pretreated zirconium English powder of the zirconium English powder stated, vanadic anhydride and sodium chloride mixing, it is thus achieved that
Mixture, is then 800 900 DEG C by described mixture constant-speed heating to temperature, and the time of described heating is
8 11h, maintaining mixture temperature is 800 900 DEG C and lasting 1 1.5h, then cools down, it is thus achieved that vanadium zirconium indigo plant
Colorant.
The preparation method of zircon-vanadium blue pigment the most according to claim 5, it is characterised in that first by described
Mixture grinds, then carries out constant-speed heating.
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| CN201810210496.3A CN108624087B (en) | 2016-01-26 | 2016-01-26 | Pretreatment method of zircon powder with high reaction activity |
| CN201810211037.7A CN108610658B (en) | 2016-01-26 | 2016-01-26 | Preparation method of low-cost vanadium-zirconium blue pigment |
| CN201610051838.2A CN105733310B (en) | 2016-01-26 | 2016-01-26 | The preprocess method of zirconium English powder and the preparation method of zircon-vanadium blue pigment |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107118589A (en) * | 2017-05-08 | 2017-09-01 | 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 |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| CN108624087B (en) | 2020-10-27 |
| CN108610658B (en) | 2020-10-27 |
| CN105733310B (en) | 2018-04-17 |
| CN108610658A (en) | 2018-10-02 |
| CN108624087A (en) | 2018-10-09 |
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