CN108083323A - The preparation method of highly pure cadmium sulfide - Google Patents
The preparation method of highly pure cadmium sulfide Download PDFInfo
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- CN108083323A CN108083323A CN201711239794.7A CN201711239794A CN108083323A CN 108083323 A CN108083323 A CN 108083323A CN 201711239794 A CN201711239794 A CN 201711239794A CN 108083323 A CN108083323 A CN 108083323A
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
- C01G11/02—Sulfides
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Abstract
This application provides a kind of preparation method of highly pure cadmium sulfide, including step：Sulfuric acid solution is added in dissolution kettle, heat and cadmium powder is added under stirring, while adds in catalyst salpeter solution, is persistently stirred to react until the dissolving of cadmium powder, then will add in cadmium sulfide reaction kettle after the solution filtering and impurity removing after reaction, and obtain cadmium sulfate solution；Hydrogen sulfide gas is passed through into cadmium sulfide reaction kettle to be reacted, after reaction through centrifuging, washing, drying, obtain cadmium sulfide initial material under stirring；Cadmium sulfide initial material is placed in tube-type atmosphere furnace and is calcined, and is continually fed into nitrogen or inert gas, is cooled down after calcination, highly pure cadmium sulfide powder is obtained through ball milling screening.The preparation method of the application is simple, and the production cycle is shorter, and advantages of nontoxic raw materials is harmless and reusable edible, can effectively reduce production cost, while obtained cadmium sulfide has preferable homogeneity and higher purity.
Description
Technical field
Preparation field more particularly to a kind of preparation method of highly pure cadmium sulfide this application involves cadmium sulfide.
Background technology
Cadmium sulfide (CdS) is the relatively stable semiconductor material with wide forbidden band of chemical property, and energy gap Eg is 2.42ev,
Molecular weight is 144.46g/mol, "dead", is slightly soluble in water and ethyl alcohol, is dissolved in acid and is highly soluble in ammonium hydroxide.CdS nano thin-films
With good light transfer characteristic, solar spectral visible region can be well matched with and have extraordinary transmission to visible ray
Rate serves as Window layer usually using CdS nano thin-films and heterojunction solar battery is formed together with p-type semiconductor material.Such as CdS
Nano thin-film can be used as n-type semiconductor layer in CIGS thin film solar cell, form p-n junction with cigs layer, form solar energy
Battery.CdS is to match best cushioning layer material with CIGS at present simultaneously, at present, by German solar energy and Hydrogen Energy research center
The highest conversion ratio of the CIGS thin film solar cell using CdS film as buffer layer of manufacture has reached 20.3%.
With flourishing for CIGS thin film solar cell, CdS is also more paid attention in the effect of field of solar energy.Together
When experimental study in find that CdS heterojunction solar batteries have many advantages, such as high-conversion rate, low cost and simple for process, therefore,
CdS will be following cheap, high efficiency solar cell development main direction of studying, play the work that Solar use is promoted to promote
With present and later energy crisis can be alleviated.Therefore, be badly in need of developing a kind of highly pure cadmium sulfide production technology of low cost with
Meet the market demand.
At present, the method for synthesizing cadmium sulfide mainly has caddy hydrogen sulfide synthetic method and gas phase synthesis method.
2 months 2008 Chinese patent application CN101125680A disclosed in 20 days disclose a kind of in aqueous solution by heavy
The method that shallow lake mode prepares highly pure cadmium sulfide specifically discloses and 5N cadmiums is dissolved in top grade pure hydrochloric acid, and chlorine is obtained through evaporating depickling
Then caddy aqueous solution is fitted into sulfide-cadmium precipitation pond by cadmium aqueous solution, 5N sulphur is fitted into graphite boat, then will be equipped with
The graphite boat of 5N sulphur is put into quartz ampoule, and one end of quartz ampoule sets hydrogen inlet, and the other end sets hydrogen sulfide outlet, and quartz ampoule is put
Enter in heating furnace, open the heating system of heating furnace, 4N hydrogen and the generation 5N vulcanizations of 5N reaction of Salmon-Saxl are then passed through by hydrogen inlet
Hydrogen is exported from hydrogen sulfide and 5N hydrogen sulfide is passed through into sulfide-cadmium precipitation pond, and reaction, which generates cadmium sulfide and precipitates, is obtained by filtration 5N sulphur
Cadmium product.Chemical reagent used in this method is more, and synthesis cycle is long, while is dissolved using hydrochloric acid as dissolution system
Hydrochloric acid volatile quantity is larger higher to equipment requirement in journey, while the reaction category reversible reaction of caddy and hydrogen sulfide, can cause to close
Reaction into cadmium sulfide is difficult to thoroughly carry out, while requirement of this method to raw material is high and raw material availability is relatively low, causes to produce
It is of high cost, and easy residual chlorine (Cl) ion in product, influence the follow-up use of cadmium sulfide.
Chinese patent application CN105060336A disclosed in 18 days November in 2015 discloses a kind of cadmium sulfide vapor- phase synthesis
Device, the method synthesizing cadmium sulfide directly reacted using gaseous state cadmium and gaseous sulfur are avoided and introduce other impurities and can make
It is standby to obtain the higher cadmium sulfide of purity.This method is simple for process, but high to equipment requirement, easily remaining in the cadmium sulfide of synthesis
React halfway simple substance cadmium and elemental sulfur, it is necessary to carry out subsequent processing (such as be evaporated in vacuo), exist simultaneously equipment investment compared with
Greatly, the problems such as controllability is relatively poor, and generation is relatively low, and production cost is higher is reacted.
In consideration of it, special propose the application.
The content of the invention
In view of problem present in background technology, the application's is designed to provide a kind of preparation side of highly pure cadmium sulfide
Method, its preparation method is simple, and the production cycle is shorter, and advantages of nontoxic raw materials is harmless and reusable edible, can effectively reduce production cost, together
When the cadmium sulfide that makes there is preferable homogeneity and higher purity.
In order to achieve the above object, this application provides a kind of preparation method of highly pure cadmium sulfide, including step：By sulphur
Acid solution is added in dissolution kettle, heats and cadmium powder is added under stirring, while adds in catalyst salpeter solution, lasting to stir
Then reaction will add in cadmium sulfide reaction kettle after the solution filtering and impurity removing after reaction until the dissolving of cadmium powder, it is molten to obtain cadmium sulfate
Liquid；Hydrogen sulfide gas is passed through into cadmium sulfide reaction kettle under stirring to be reacted, after reaction through centrifuging, washing,
It is dry, obtain cadmium sulfide initial material；Cadmium sulfide initial material is placed in tube-type atmosphere furnace and is calcined, and is continually fed into nitrogen or indifferent gas
Body cools down after calcination, and highly pure cadmium sulfide powder is obtained through ball milling screening.
Compared with the prior art, the application includes at least advantageous effect as described below：
The application prepares cadmium sulfate solution using nitric acid as catalyst and derivant, using cadmium powder and sulfuric acid as raw material, this mistake
Journey reaction speed is very fast, can significantly shorten the production cycle, and has the advantages that vent gas treatment is at low cost, safety and environmental protection.
The application produces the process of cadmium sulfide under normal temperature condition using cadmium sulfate solution and stink damp precursor reactant
It carries out, obtained cadmium sulfide homogeneity is good, and the sulfuric acid system of simultaneous reactions process middle and high concentration also makes cadmium sulfide with higher
Purity, and the solution the isolated after reaction still sulfuric acid containing higher amount may continue as feedstock circulation utilization.
The method that the application prepares high-purity cadmium sulfide has single batch of production capacity big, is easy to the advantages such as industrialization, meets vulcanization
Cadmium market high-purity, low cost, developing direction simple for process.
Specific embodiment
The following detailed description of the preparation method of the highly pure cadmium sulfide of the application.
Step is included according to the preparation method of the highly pure cadmium sulfide of the application：Sulfuric acid solution is added in dissolution kettle, added by S1
Heat simultaneously adds in cadmium powder under stirring, while adds in catalyst salpeter solution, is persistently stirred to react until cadmium powder dissolves, then
It will be added in after solution filtering and impurity removing after reaction to cadmium sulfide reaction kettle, obtain cadmium sulfate solution；S2, to sulphur under stirring
Hydrogen sulfide gas is passed through in cadmium reaction kettle to be reacted, and after reaction through centrifuging, washing, drying, obtains cadmium sulfide initial material；
Cadmium sulfide initial material is placed in tube-type atmosphere furnace and calcines by S3, and is continually fed into nitrogen or inert gas, cools down after calcination,
Highly pure cadmium sulfide powder is obtained through ball milling screening.
In the preparation method according to highly pure cadmium sulfide described herein, using nitric acid as catalyst and derivant, with
Cadmium powder and sulfuric acid prepare cadmium sulfate solution for raw material, and reaction equation is as shown in Equation 1, this reaction speed is very fast, can significantly contract
Short production cycle, and there is the advantages of rate of dissolution is fast, and vent gas treatment is at low cost, safety and environmental protection.Cadmium sulfate solution and hydrogen sulfide
The reaction equation that gas reaction prepares cadmium sulfide is as shown in Equation 2, can be carried out under this process normal temperature condition, obtained cadmium sulfide
Homogeneity is good, and the sulfuric acid system of simultaneous reactions process middle and high concentration also makes cadmium sulfide have higher purity, divides after reaction
The solution separated out the still sulfuric acid containing higher amount may continue as feedstock circulation utilization.The high-purity vulcanization of the application
The preparation method of cadmium has single batch of production capacity big, is easy to the advantages such as industrialization, meets cadmium sulfide market high-purity, low cost, technique
Simple developing direction.
CdSO4+H2S→CdS↓+H2SO4Formula 2
In the preparation method according to highly pure cadmium sulfide described herein, in step S1, the purity of the cadmium powder is more than
Equal to 5N, the grain size of the cadmium powder is less than or equal to 325 μm.
In the preparation method according to highly pure cadmium sulfide described herein, in step S1, dissolution kettle can be glass kettle etc.
The reaction kettle of sulfuric acid corrosion resistant.
In the preparation method according to highly pure cadmium sulfide described herein, in step S1, the purity of salpeter solution is change
Learn it is pure and more than, the purity of sulfuric acid solution for chemistry it is pure and more than.
In the preparation method according to highly pure cadmium sulfide described herein, in step S1, the mass fraction of salpeter solution
More than or equal to 20%.It is unsuitable too fast to add in the speed of salpeter solution, is advisable with not generating nitrogen oxides.Preferably, using dropwise addition
Mode add in salpeter solution.
In the preparation method according to highly pure cadmium sulfide described herein, in step S1, nitric acid, the mass ratio of cadmium powder are
(5~40):100, wherein, the quality of nitric acid refers to the Solute mass of salpeter solution.
In the preparation method according to highly pure cadmium sulfide described herein, in step S1, the mass fraction of sulfuric acid solution
More than or equal to 20%.Sulfuric acid solution can be directly using the relatively low dilute sulfuric acid of commercial available quality fraction, can also be by diluting quality
The higher concentrated sulfuric acid of fraction higher, purity (mass fraction be more than 70%) obtains, wherein, during dilution it is preferable to use distilled water, go
Ionized water or purified water.
In the preparation method according to highly pure cadmium sulfide described herein, in step S1, sulfuric acid, cadmium powder mass ratio can
For (85~105):100, wherein, the quality of sulfuric acid refers to the Solute mass of sulfuric acid solution.
In the preparation method according to highly pure cadmium sulfide described herein, in step S1, the temperature for heating reaction is 70
DEG C~150 DEG C, it is preferable that the temperature for heating reaction is 90 DEG C~120 DEG C.
In the preparation method according to highly pure cadmium sulfide described herein, in step S1, steaming can be added in after reaction
The cadmium sulfate solution that distilled water, deionized water or purified water dilute, diluted purpose are that the cadmium sulfate solution prevented is cold
But there is crystal precipitation during, this step can also be omitted, as long as ensureing that obtained cadmium sulfate solution is not up at normal temperatures
Hypersaturated state.
In the preparation method according to highly pure cadmium sulfide described herein, in step S1, the purpose of filtering and impurity removing is to remove
Remove the complete cadmium powder of unreacted and the impurity insoluble in sulfuric acid.The species of the filter used during filtering and impurity removing is not specific
Limitation, can make choice according to actual demand.Specifically, filter may be selected from bag filter or filter cartridge type filter.
In the preparation method according to highly pure cadmium sulfide described herein, in step S2, the purity of hydrogen sulfide is more than etc.
In 3N.
In the preparation method according to highly pure cadmium sulfide described herein, in step S2, hydrogen sulfide can be leaned on from reaction kettle
The position of nearly bottom is passed through, and is passed through rate and is not limited specifically, can be made choice according to actual conditions, it is preferable that hydrogen sulfide
The rate that is passed through can be 1L/min~3L/min.
In the preparation method according to highly pure cadmium sulfide described herein, in step S2, when reaction, into solution, cadmium contains
When amount is less than 20g/L, stopping is passed through hydrogen sulfide, and reaction was completed.
In the preparation method according to highly pure cadmium sulfide described herein, in step S2, centrifuge Mother liquor it is main into
Point it is substantial amounts of high-concentration sulfuric acid and a small amount of unreacted cadmium sulfate, therefore mother liquor is recyclable makes for dissolving cadmium powder cycle
With.
In the preparation method according to highly pure cadmium sulfide described herein, in step S2, the mode of washing is not specific
Limitation, can be made choice according to actual demand.It specifically, can be with distilled water, deionized water or purified water to consolidating after centrifugation
Body ingredient is washed.
In the preparation method according to highly pure cadmium sulfide described herein, in step S3, cadmium sulfide initial material is placed in stone
In Ying Zhou, then quartz boat is put into the quartz ampoule for be placed in tube-type atmosphere furnace and calcined.Wherein, cadmium sulfide initial material is placed in
After in quartz boat, nitrogen or inert gas are passed through to exhaust extra oxygen, are also required to lasting be passed through nitrogen in calcination process
Or inert gas, the vapor generated in reaction process is discharged.
In the preparation method according to highly pure cadmium sulfide described herein, in step S3, calcining heat for 200 DEG C~
600 DEG C, it is preferable that calcining heat is 250 DEG C~400 DEG C.Calcination time can be more than or equal to 2h, it is preferable that calcination time 2h
~8h.
In the preparation method according to highly pure cadmium sulfide described herein, in step S3, the mode and ball grinder of ball milling
Species do not limit specifically, can be made choice according to actual demand, specifically, ball grinder may be selected from polyurethane ball-milling pot or
Zirconia ball grinding jar.
With reference to embodiment, the application is expanded on further.It is to be understood that these embodiments be merely to illustrate the application without
For limiting scope of the present application.
Embodiment 1
35L purified waters are added in into 50L laminated glass kettles, are then turned on stirring, are slowly added to (the analysis of the 8.9kg concentrated sulfuric acids
Pure, mass fraction 98%, blunting of attention adds in, and prevents bumping), it then opens and is heated to 80 DEG C ± 5 DEG C, in stirring shape
10kg mesh numbers are added portionwise under state as the 5N cadmium powder below 100 mesh, at the same be added dropwise into glass kettle 0.77kg nitric acid (chemistry is pure,
Mass fraction is that 65%), insulated and stirred is to pH >=1 of solution after the completion of charging, and after reaction plus purified water is settled to 30L,
Then solution is added in cadmium sulfide reaction kettle by bag filter, obtaining limpid cadmium sulfate solution, (wherein, cadmium is dense
Degree is about 330g/L).
Cadmium sulfide stirring apparatus for reaction kettle is opened, it is pure from being passed through close to the position of bottom with the rate of 1L/min~3L/min
It spends and is reacted for the hydrogen sulfide gas of 4N, stop being passed through stink damp when the concentration of reaction cadmium into solution is less than 20g/L
Body, reaction was completed, is then centrifuged, mother liquor (sulfuric acid containing higher concentration and unreacted cadmium sulfate, sulphur after centrifugation
The concentration of acid is about 280g/L) glass kettle recycling is transferred to, then the purifying water washing of the solid constituent after centrifugation dries
Discharging obtains cadmium sulfide initial material.
Cadmium sulfide initial material is contained with quartz boat, is then put into quartz boat in the quartz ampoule for being placed in tube-type atmosphere furnace, with 2L/
The rate of min is passed through nitrogen so that the oxygen in quartz ampoule to be discharged, then heating calcining, be continually fed into calcination process nitrogen with
Vapor is discharged, wherein, the temperature of calcining is 200 DEG C, and the time of calcining is 8h, after being cooled to less than 80 DEG C after calcination
Then discharging obtains 12.2kg cadmium sulfides after ball milling screening, the yield of cadmium sulfide is 94.9%, sampling analysis, cadmium sulfide it is pure
Degree reaches 5N.
Embodiment 2
30L purified waters are added in into 50L laminated glass kettles, are then turned on stirring, the 10.68kg concentrated sulfuric acids is slowly added to and (changes
Pure, mass fraction 98% is learned, blunting of attention adds in, and prevents bumping), it then opens and is heated to 100 DEG C ± 5 DEG C, stirring
It mixes and 10kg mesh numbers is added portionwise under state as the 5N cadmium powder below 200 mesh, while (the analysis of 6.1kg nitric acid is added dropwise into glass kettle
It is pure, mass fraction 65%), insulated and stirred is to pH >=0.5 of solution after the completion of charging, and after reaction plus purified water is settled to
Then solution by filter cartridge type filter is added in cadmium sulfide reaction kettle and obtains limpid cadmium sulfate solution (wherein, cadmium by 40L
Concentration be about 50g/L).
The agitating device of cadmium sulfide reaction kettle is opened, is passed through from the position close to bottom with the rate of 1L/min~3L/min
Purity is that the hydrogen sulfide gas of 4N is reacted, and stops being passed through hydrogen sulfide when the concentration of reaction cadmium into solution is less than 10g/L
Gas, reaction was completed, is then centrifuged, mother liquor after centrifugation (sulfuric acid containing higher concentration and unreacted cadmium sulfate,
The concentration of sulfuric acid is about 220g/L) it is transferred to glass kettle recycling, solid constituent after centrifugation is dried with after purifying water washing
Discharging obtains cadmium sulfide initial material.
Cadmium sulfide initial material is contained with quartz boat, is then put into quartz boat in the quartz ampoule for being placed in tube-type atmosphere furnace, with 6L/
The speed of min is passed through argon gas and discharges the oxygen in quartz ampoule, then heating calcining, and argon gas is continually fed into calcination process to incite somebody to action
Vapor is discharged, and the temperature of calcining is 600 DEG C, and the time of calcining is 2h, discharging after being cooled to less than 80 DEG C after calcination, so
12.43kg cadmium sulfides are obtained after ball milling screening afterwards, the yield of cadmium sulfide is 96.7%, and sampling analysis, the purity of cadmium sulfide reaches
5N。
Embodiment 3
30L purified waters are added in into 50L laminated glass kettles, is then turned on stirring, is slowly added to the 9.79kg concentrated sulfuric acid (top grades
Pure, mass fraction 98%, blunting of attention adds in, and prevents bumping), it then opens and is heated to 120 DEG C ± 5 DEG C, in stirring
Under 10kg mesh numbers are added portionwise as the 5N cadmium powder below 325 mesh, while 3.1kg nitric acid (top pure grade, quality are added dropwise into reaction kettle
Fraction is that 65%), insulated and stirred is to pH >=0.5 of solution after the completion of charging, and after reaction plus water is settled to 50L, Ran Houtong
It crosses bag filter and adds in solution and to cadmium sulfide reaction kettle, obtain limpid cadmium sulfate solution (wherein, the concentration of cadmium is about
200g/L)。
The agitating device of cadmium sulfide reaction kettle is opened, is passed through from the position close to bottom with the rate of 1L/min~3L/min
Hydrogen sulfide gas, which is reacted, to be stopped being passed through hydrogen sulfide gas when the concentration of cadmium in solution is less than 5g/L, and reaction was completed, then
It is centrifuged, (sulfuric acid containing higher concentration and unreacted cadmium sulfate, the concentration of sulfuric acid are about the mother liquor after centrifugation
Glass kettle recycling 190g/L) is transferred to, the solid constituent after centrifugation obtains cadmium sulfide with discharging is dried after purifying water washing
Initial material.
Cadmium sulfide initial material is contained with quartz boat, is then put into quartz boat in the quartz ampoule for being placed in tube-type atmosphere furnace, with 6L/
The speed of min is passed through argon gas and discharges the oxygen in quartz ampoule, then heating calcining, and argon gas is continually fed into calcination process to incite somebody to action
Vapor is discharged, and the temperature of calcining is 300 DEG C, and the time of calcining is 4h, and discharging is right after being cooled to less than 80 DEG C after calcination
12.5kg cadmium sulfides are obtained after ball milling screening afterwards, the yield of cadmium sulfide is 97.28%, and sampling analysis, the purity of cadmium sulfide reaches
5N。
Claims (10)
1. a kind of preparation method of highly pure cadmium sulfide, which is characterized in that including step：
S1 adds in sulfuric acid solution in dissolution kettle, heats and cadmium powder is added under stirring, while it is molten to add in catalyst nitric acid
Liquid is persistently stirred to react until the dissolving of cadmium powder, then will add in cadmium sulfide reaction kettle after the solution filtering and impurity removing after reaction, obtain
To cadmium sulfate solution；
S2, under stirring being passed through hydrogen sulfide gas into cadmium sulfide reaction kettle is reacted, after reaction through centrifuging, washing
It washs, dry, obtain cadmium sulfide initial material；
Cadmium sulfide initial material is placed in tube-type atmosphere furnace and calcines by S3, and is continually fed into nitrogen or inert gas, drops after calcination
Temperature obtains highly pure cadmium sulfide powder through ball milling screening.
2. the preparation method of highly pure cadmium sulfide according to claim 1, which is characterized in that in step S1, the cadmium powder
Purity is more than or equal to 5N；The grain size of the cadmium powder is less than or equal to 325 μm.
3. the preparation method of highly pure cadmium sulfide according to claim 1, which is characterized in that in step S1, salpeter solution
Mass fraction is more than or equal to 20%.
4. the preparation method of highly pure cadmium sulfide according to claim 1, which is characterized in that in step S1, nitric acid, cadmium powder
Mass ratio is (5~40):100.
5. the preparation method of highly pure cadmium sulfide according to claim 1, which is characterized in that in step S1, sulfuric acid solution
Mass fraction is more than or equal to 20%.
6. the preparation method of highly pure cadmium sulfide according to claim 1, which is characterized in that in step S1, sulfuric acid, cadmium powder
Mass ratio is (85~105):100.
7. the preparation method of highly pure cadmium sulfide according to claim 1, which is characterized in that in step S1, heat reaction
Temperature is 70 DEG C~150 DEG C, it is preferable that the temperature for heating reaction is 90 DEG C~120 DEG C.
8. the preparation method of highly pure cadmium sulfide according to claim 1, which is characterized in that in step S3, calcining heat is
200 DEG C~600 DEG C, it is preferable that calcining heat is 250 DEG C~400 DEG C.
9. the preparation method of highly pure cadmium sulfide according to claim 1, which is characterized in that in step S3, calcination time is big
In equal to 2h, it is preferable that calcination time is 2h~8h.
10. the preparation method of highly pure cadmium sulfide according to claim 1, which is characterized in that, will be at the beginning of cadmium sulfide in step S3
Material is placed in quartz boat, is then put into quartz boat in the quartz ampoule for be placed in tube-type atmosphere furnace and is calcined.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113511671A (en) * | 2021-04-14 | 2021-10-19 | 广东先导稀材股份有限公司 | Production method of high-purity one-third cadmium sulfate octahydrate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125680A (en) * | 2007-08-31 | 2008-02-20 | 侯仁义 | Method for preparing highly pure cadmium sulfide |
-
2017
- 2017-11-30 CN CN201711239794.7A patent/CN108083323A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125680A (en) * | 2007-08-31 | 2008-02-20 | 侯仁义 | Method for preparing highly pure cadmium sulfide |
Non-Patent Citations (1)
| Title |
|---|
| 大貫等: "Piperの方法によるCdS結晶の生成", 《日本物理学会誌》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113511671A (en) * | 2021-04-14 | 2021-10-19 | 广东先导稀材股份有限公司 | Production method of high-purity one-third cadmium sulfate octahydrate |
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Effective date of registration: 20181121 Address after: 511517 D Workshop of Qingyuan Pioneer Materials Co., Ltd. No. 27-9 Baijia Industrial Park, Qingyuan High-tech Zone, Guangdong Province Applicant after: Pilot film material (Guangdong) Co., Ltd. Address before: 511517 Qingyuan 27-9 high tech Industrial Park, Guangdong Applicant before: Qingyuan Xiandao Materials Co., Ltd. |
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Application publication date: 20180529 |
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| RJ01 | Rejection of invention patent application after publication |