CN112374524A - Preparation method of cerium dioxide nano powder based on dry tremella - Google Patents

Preparation method of cerium dioxide nano powder based on dry tremella Download PDF

Info

Publication number
CN112374524A
CN112374524A CN202011414255.4A CN202011414255A CN112374524A CN 112374524 A CN112374524 A CN 112374524A CN 202011414255 A CN202011414255 A CN 202011414255A CN 112374524 A CN112374524 A CN 112374524A
Authority
CN
China
Prior art keywords
cerium
tremella
dry
pieces
lugs
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202011414255.4A
Other languages
Chinese (zh)
Inventor
焦钰
狄玉丽
张万明
张�浩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xichang College
Original Assignee
Xichang College
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xichang College filed Critical Xichang College
Priority to CN202011414255.4A priority Critical patent/CN112374524A/en
Publication of CN112374524A publication Critical patent/CN112374524A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/206Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • C01F17/224Oxides or hydroxides of lanthanides
    • C01F17/235Cerium oxides or hydroxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/10Preparation or treatment, e.g. separation or purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Cosmetics (AREA)

Abstract

The invention discloses a preparation method of cerium dioxide nano powder based on dry tremella, which comprises the following steps: dissolving cerium salt in water to prepare a cerium salt solution; weighing dry silver lugs, and adding the dry silver lugs into a cerium salt solution for swelling; and (3) washing the swelled tremella pieces, drying in an oven or freeze drying, and calcining in a muffle furnace to obtain the cerium dioxide nano powder based on the dried tremella. The method is simple, controllable, low in cost and suitable for industrial production, and can effectively improve the additional value of the cerium dioxide.

Description

Preparation method of cerium dioxide nano powder based on dry tremella
Technical Field
The invention belongs to the technical field of rare earth material application, and particularly relates to a preparation method of cerium dioxide nano powder based on dry tremella.
Background
In rare earth, the price of cerium is low, the 99.9 percent of cerium oxide in 2020 is only about 13 yuan/kg, the price of nano cerium oxide is generally 100 yuan/kg or more, and the nano cerium oxide is beneficial to improving the added value of the cerium oxide. The existing method for preparing nano powder comprises the following steps: 1. gas phase method: the common methods include inert gas condensation, sputtering, vacuum vapor deposition on a flowing liquid surface, energization heating, wire explosion, chemical vapor reaction, and the like. 2. Liquid phase method: precipitation methods, hydrolysis methods, hydrothermal methods, spraying methods, sol-gels, and the like are common. 3. Solid phase method: the thermal decomposition method, the solid phase reaction method, the spark discharge method, the dissolution method, the ball milling method, etc. are commonly used.
The preparation method of the nano cerium dioxide mainly comprises a precipitation method, a hydrothermal method and a sol-gel method. Wherein, the technological conditions (dripping speed and reaction temperature) for preparing the nano cerium dioxide by the precipitation method are difficult to control, the reaction time is long, and the particle size distribution of the prepared powder is wide; the hydrothermal method for preparing the nano cerium dioxide has long reaction time and complex process; the sol-gel method for preparing the nano cerium dioxide has long reaction time, complex process and large particle size of the prepared powder.
The prior literature reports that the template agent is obtained by treating petals, eggshell inner membrane and the like with acid and alkali or by calcining starch and glucose at high temperature. Precipitating a cerium source in a template agent in a solution, drying and calcining to obtain the nano cerium dioxide. The methods obtain the template agent through pretreatment, and simultaneously need to add a precipitator, and then obtain the nano cerium dioxide through drying and calcining.
Therefore, there is a need for a novel method for preparing cerium dioxide nanopowder.
Disclosure of Invention
In view of the above, the invention provides a preparation method of cerium dioxide nano powder based on dry tremella aiming at the problems of complex process, long time consumption and high production cost.
In order to solve the technical problem, the invention discloses a preparation method of cerium dioxide nano powder based on dry tremella, which comprises the following steps:
step 1, preparing a cerium salt solution: dissolving cerium salt in water to prepare a cerium salt solution;
step 2, weighing dry silver lugs, and adding the dry silver lugs into a cerium salt solution for swelling; and (3) washing the swelled tremella pieces, drying in an oven or freeze drying, and calcining in a muffle furnace to obtain the cerium dioxide nano powder based on the dried tremella.
Optionally, the cerium salt in step 1 is one of cerium nitrate, cerium sulfate or cerium acetate.
Optionally, the dissolution temperature in step 1 is 50 ℃ to 80 ℃.
Optionally, the mass ratio of the cerium salt to the water in the step 1 is 1:1-1: 10.
Optionally, the dry tremella pieces in the step 2 account for 5-50% of the total mass of the cerium salt.
Optionally, the swelling rotation speed in the step 2 is 50-150r/min, and the swelling time is 0.5-1.5 h.
Optionally, the oven drying time in the step 2 is 1.5-2.5 h, and the oven drying temperature is 75-85 ℃.
Optionally, the freeze-drying time in the step 2 is 1.5-2.5 h, and the freeze-drying temperature is-25 ℃ to-40 ℃.
Alternatively, the calcination temperature in step 2 is 550 ℃ to 1050 ℃.
Compared with the prior art, the invention can obtain the following technical effects:
1) the nano cerium dioxide prepared by the invention can be widely applied to photocatalytic materials, cerium dioxide polishing powder materials, glass industrial additives, cosmetic ultraviolet absorbers and the like.
2) The method is simple, controllable, low in cost and suitable for industrial production, and can effectively improve the additional value of the cerium dioxide.
Of course, it is not necessary for any one product in which the invention is practiced to achieve all of the above-described technical effects simultaneously.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is an XRD diffraction pattern of dried tremella-based cerium dioxide nanopowder prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of dried tremella-based cerium dioxide nanopowder prepared in example 1 of the present invention;
fig. 3 is a diffuse reflection spectrum of the cerium dioxide nano powder based on dry tremella prepared in example 1 of the present invention.
Detailed Description
The following embodiments are described in detail with reference to the accompanying drawings, so that how to implement the technical features of the present invention to solve the technical problems and achieve the technical effects can be fully understood and implemented.
The invention discloses a preparation method of cerium dioxide nano powder based on dry tremella, which comprises the following steps:
step 1, preparing a cerium salt solution: dissolving cerium salt in water at the temperature of 50-80 ℃ according to the mass ratio of 1:1-10 to prepare a cerium salt solution; wherein, the cerium salt is one of cerium nitrate, ammonium ceric nitrate, cerium sulfate or cerium acetate;
wherein, nitrate salt, sulfate salt and acetate salt can be decomposed at high temperature to generate oxide, if the oxide is directly decomposed at high temperature, the particle size of the generated oxide is extremely large and often reaches micron level, and the nano effect of materials is avoided. When preparing the nano oxide material, the nano oxide is generally sintered by utilizing the morphology inheritance of the precipitate which is generated in advance, such as nano hydroxide, nano oxalate, nano carbonate and the like, and is sintered at high temperature. According to the method, a precipitator is not added, the tremella fuciformis slices are used as templates, and the solution of cerium nitrate, cerium sulfate, cerium acetate and ammonium cerium nitrate is directly calcined to prepare the nano cerium oxide.
Step 2, weighing dry silver lugs, wherein the dry silver lugs account for 5-50% of the mass of the cerium salt solution, and adding the dry tremella lugs into the cerium salt solution at a rotating speed of 50-150r/min to swell for 0.5-1.5 h; and (3) after the swelled tremella pieces are washed, drying the tremella pieces in an oven at the temperature of 75-85 ℃ for 1.5-2.5 h or freeze-drying the tremella pieces at the temperature of-25 ℃ to-40 ℃ for 1.5-2.5 h, and calcining the tremella pieces in a muffle furnace at the temperature of 550-1050 ℃ to prepare the cerium dioxide nano powder based on the dry tremella.
Wherein, the calcining temperature is lower than 550 ℃ and can not decompose nitrate radical, sulfate radical and acetate radical, the sintering temperature is too high and exceeds 1050 ℃, the size of the produced powder is enlarged, and simultaneously, the energy consumption is too high.
The ratio of the solution to the silver lug is too high, the tremella fuciformis can not completely absorb the solution, the ratio of the solution to the silver lug is too low, and the tremella fuciformis is wasted greatly.
Example 1
Dissolving cerium nitrate in water according to the mass ratio of 1:5 at the temperature of 65 ℃ to prepare a cerium nitrate solution; weighing dry silver lugs, wherein the dry silver lugs account for 30% of the total mass of the cerous nitrate solution, and adding the dry tremella pieces into the cerous nitrate solution at the rotating speed of 100 r/min to swell for 2 hours; and (3) washing the swelled tremella pieces, drying the tremella pieces in an oven at 80 ℃ for 2h, and calcining the tremella pieces in a muffle furnace at 800 ℃ to obtain the cerium dioxide nano powder based on the dried tremella.
Example 2
Dissolving ammonium ceric nitrate in water at the temperature of 50 ℃ according to the mass ratio of 1:10 to prepare ammonium ceric nitrate solution; weighing dry silver lugs, wherein the dry silver lugs account for 5% of the mass of the ammonium ceric nitrate solution, and adding the dry tremella pieces into the ammonium ceric nitrate solution at the rotating speed of 150r/min to swell for 0.5 h; and (3) washing the swelled tremella pieces, drying the tremella pieces in an oven at 85 ℃ for 1.5h, and calcining the tremella pieces in a muffle furnace at 1050 ℃ to obtain the cerium dioxide nano powder based on the dried tremella.
Example 3
Dissolving cerium sulfate in water according to the mass ratio of 1:1 at the temperature of 80 ℃ to prepare a cerium sulfate solution; weighing dry silver lugs, wherein the dry silver lugs account for 50% of the total mass of the cerium sulfate solution, and adding the dry tremella pieces into the cerium sulfate solution at a rotating speed of 50r/min to swell for 1.5 h; and (3) washing the swelled tremella pieces, drying the tremella pieces in a 75 ℃ oven for 2.5 h, and calcining the tremella pieces in a muffle furnace at 550 ℃ to obtain the cerium dioxide nano powder based on the dried tremella.
Example 4
Dissolving cerium acetate in water according to the mass ratio of 1:3 at the temperature of 60 ℃ to prepare a cerium acetate solution; weighing dry silver lugs, wherein the dry silver lugs account for 10% of the total mass of the cerium acetate solution, and adding the dry tremella pieces into the cerium acetate solution at a rotating speed of 120 r/min to swell for 0.8 h; and (3) washing the swelled tremella pieces, drying the tremella pieces in an oven at 78 ℃ for 2.2 h, and calcining the tremella pieces in a muffle furnace at 750 ℃ to obtain the cerium dioxide nano powder based on the dried tremella.
Example 5
Dissolving cerium nitrate in water according to the mass ratio of 1:8 at the temperature of 70 ℃ to prepare a cerium nitrate solution; weighing dry silver lugs, wherein the dry silver lugs account for 40% of the total mass of the cerous nitrate solution, and adding the dry tremella pieces into the cerous nitrate solution at a rotating speed of 80 r/min to swell for 1.2 h; and (3) washing the swelled tremella pieces, then carrying out freeze drying for 2h at the temperature of-30 ℃, and calcining at the temperature of 850 ℃ in a muffle furnace to prepare the cerium dioxide nano powder based on the dried tremella.
Example 6
Dissolving ammonium ceric nitrate in water according to the mass ratio of 1:6 at the temperature of 55 ℃ to prepare ammonium ceric nitrate solution; weighing dry silver lugs, wherein the dry silver lugs account for 30% of the total mass of the ammonium ceric nitrate solution, and adding the dry tremella pieces into the ammonium ceric nitrate solution at the rotating speed of 90 r/min to swell for 1.5 h; and (3) washing the swelled tremella pieces, freeze-drying at-25 ℃ for 1.5h, and calcining at 550 ℃ in a muffle furnace to obtain the cerium dioxide nano powder based on the dried tremella.
Example 7
Dissolving cerium sulfate in water according to the mass ratio of 1:4 at the temperature of 75 ℃ to prepare a cerium sulfate solution; weighing dry silver lugs, wherein the dry silver lugs account for 35% of the total mass of the cerium sulfate solution, and adding the dry tremella pieces into the cerium sulfate solution at a rotating speed of 80 r/min to swell for 1.1 h; and (3) washing the swelled tremella pieces, then carrying out freeze drying at-40 ℃ for 2.5 h, and calcining at 950 ℃ in a muffle furnace to obtain the cerium dioxide nano powder based on the dried tremella.
Example 8
Dissolving cerium acetate in water according to the mass ratio of 1:5 at the temperature of 65 ℃ to prepare a cerium acetate solution; weighing dry silver lugs, wherein the dry silver lugs account for 25% of the total mass of the cerium acetate solution, and adding the dry tremella pieces into the cerium acetate solution at a rotating speed of 100 r/min to swell for 1 h; and (3) washing the swelled tremella pieces, then carrying out freeze drying at-35 ℃ for 2h, and calcining at 1050 ℃ in a muffle furnace to obtain the cerium dioxide nano powder based on the dried tremella.
As can be seen from FIG. 1, the XRD diffraction pattern of the dried tremella-based cerium dioxide nano-powder prepared in example 1 is compared with the standard cerium dioxide PDF card #81-0792, so that the product after calcination has no impurities, cerium oxide is generated, and the product has high crystallinity. As can be seen from fig. 2, the scanning electron microscope image of the dried tremella-based ceria nano-powder prepared in example 1 shows that the prepared ceria has good dispersibility, the particle size of the product is less than 100 nm, and a large amount of nano-powder is aggregated together to form the porous material. As can be seen from FIG. 3, when the cerium dioxide prepared by Colon is used as a reference, the diffuse reflection spectrum of the nano cerium dioxide prepared in example 1 at the wavelength of 200-800 nm is determined, and the ultraviolet absorption of the sample is obviously improved.
While the foregoing description shows and describes several preferred embodiments of the invention, it is to be understood, as noted above, that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (9)

1. A preparation method of cerium dioxide nano powder based on dry tremella is characterized by comprising the following steps:
step 1, preparing a cerium salt solution: dissolving cerium salt in water to prepare a cerium salt solution;
step 2, weighing dry silver lugs, and adding the dry silver lugs into a cerium salt solution for swelling; and (3) washing the swelled tremella pieces, drying in an oven or freeze drying, and calcining in a muffle furnace to obtain the cerium dioxide nano powder based on the dried tremella.
2. The method according to claim 1, wherein the cerium salt in step 1 is one of cerium nitrate, cerium sulfate or cerium acetate.
3. The method according to claim 1, wherein the dissolution temperature in the step 1 is 50 ℃ to 80 ℃.
4. The method according to claim 1, wherein the cerium salt and water in step 1 are in a mass ratio of 1:1 to 1: 10.
5. The preparation method according to claim 1, wherein the dry tremella pieces in the step 2 account for 5-50% of the cerium salt by mass.
6. The preparation method according to claim 1, wherein the swelling speed in step 2 is 50-150r/min, and the swelling time is 0.5-1.5 h.
7. The preparation method according to claim 1, wherein the oven drying time in the step 2 is 1.5-2.5 h, and the oven drying temperature is 75-85 ℃.
8. The method according to claim 1, wherein the freeze-drying time in step 2 is 1.5 to 2.5 hours, and the freeze-drying temperature is-25 ℃ to-40 ℃.
9. The method according to claim 1, wherein the calcination temperature in the step 2 is 550 ℃ to 1050 ℃.
CN202011414255.4A 2020-12-07 2020-12-07 Preparation method of cerium dioxide nano powder based on dry tremella Pending CN112374524A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011414255.4A CN112374524A (en) 2020-12-07 2020-12-07 Preparation method of cerium dioxide nano powder based on dry tremella

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011414255.4A CN112374524A (en) 2020-12-07 2020-12-07 Preparation method of cerium dioxide nano powder based on dry tremella

Publications (1)

Publication Number Publication Date
CN112374524A true CN112374524A (en) 2021-02-19

Family

ID=74589765

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011414255.4A Pending CN112374524A (en) 2020-12-07 2020-12-07 Preparation method of cerium dioxide nano powder based on dry tremella

Country Status (1)

Country Link
CN (1) CN112374524A (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101249952A (en) * 2008-03-27 2008-08-27 上海交通大学 Method for preparing self-doping nitrogen grading porous oxide by using biomass template
CN103818943A (en) * 2014-02-18 2014-05-28 常州大学 Spherical cerium oxide porous abrasive and its use in ultra-precision polishing
CN103920486A (en) * 2014-03-10 2014-07-16 苏州科技学院相城研究院 Method for preparing multi-component cerium oxide based nanometer slice material
CN106006702A (en) * 2016-05-20 2016-10-12 济南大学 Bead-chain type CeO2 nanometer material and preparation method thereof
WO2019171255A1 (en) * 2018-03-05 2019-09-12 Qatar University Nanoporous cerium oxide with interconnected pores for catalysis and a cost-effective method of preparing thereof
CN111545169A (en) * 2020-05-19 2020-08-18 西南科技大学 Method for preparing hypha/molybdenum oxide adsorption-catalysis material by utilizing biological enrichment

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101249952A (en) * 2008-03-27 2008-08-27 上海交通大学 Method for preparing self-doping nitrogen grading porous oxide by using biomass template
CN103818943A (en) * 2014-02-18 2014-05-28 常州大学 Spherical cerium oxide porous abrasive and its use in ultra-precision polishing
CN103920486A (en) * 2014-03-10 2014-07-16 苏州科技学院相城研究院 Method for preparing multi-component cerium oxide based nanometer slice material
CN106006702A (en) * 2016-05-20 2016-10-12 济南大学 Bead-chain type CeO2 nanometer material and preparation method thereof
WO2019171255A1 (en) * 2018-03-05 2019-09-12 Qatar University Nanoporous cerium oxide with interconnected pores for catalysis and a cost-effective method of preparing thereof
CN111545169A (en) * 2020-05-19 2020-08-18 西南科技大学 Method for preparing hypha/molybdenum oxide adsorption-catalysis material by utilizing biological enrichment

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王炜等: "利用竹叶模板合成分级多孔CeO_2材料及其性能", 《中国有色金属学报》 *
钱君超等: "生物鸡蛋内膜结构氧化铈材料的合成与表征", 《高等学校化学学报》 *

Similar Documents

Publication Publication Date Title
CN106866142B (en) The production method of nanoscale high-purity zirconium dioxide composite granule
CN111960464B (en) Black titanium dioxide optical nano material rich in oxygen vacancy defects and preparation method and application thereof
CN109019656B (en) Method for producing nano rare earth oxide powder
CN110194480B (en) Nano cerium oxide and preparation method thereof
CN110975795A (en) Synthesis method of lithium extraction adsorbent
TWI703091B (en) Fine titanium oxide particles and method for producing same
CN102295304A (en) Preparation method of pseudo-boehmite and microcrystalline corundum abrasive
CN1597097A (en) Preparation method of high specific surface tantalate and niobate photo catalyst
JP2002255515A (en) Production method for metal oxide fine particle
CN113224380B (en) Solid electrolyte material, preparation method thereof and battery
CN104944471A (en) Tungsten doped bronze powder having high infrared shielding property and synthesis method of doped tungsten bronze powder
KR20030075992A (en) Indium oxide powder, manufacturing method thereof, and manufacturing method of high density indium tin oxide target using the same
CN105016382A (en) Method for preparing pure gold redstone type titanium dioxide nanorod
JP5233007B2 (en) Paint for transparent conductive material and method for producing transparent conductive film
CN103318949A (en) Low temperature solid phase preparation method of indium tin oxide nano particle powder
CN112374524A (en) Preparation method of cerium dioxide nano powder based on dry tremella
CN113149067A (en) Zinc orthotitanate powder and preparation method thereof
CN112744853A (en) Method for preparing cerium dioxide material for photocatalysis based on sterculia lychnophora
CN106925260B (en) Ag2O-cluster intercalated titanium oxide and preparation method and application thereof
Fan et al. Facile synthesis of urchin-like Cs x WO 3 particles with improved transparent thermal insulation using bacterial cellulose as a template
JPS60176968A (en) Manufacture of sno2-zro2-tio2 dielectric
JPH06227815A (en) Production of electrically conductive fine powder
JP5434665B2 (en) Method for producing metal oxide nanoparticles
KR100504937B1 (en) A process for producing ceo2 nano particles having a controlled particle size
KR100523451B1 (en) Production Method of Nano-sized Crystalline Titania Powders

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20210219

RJ01 Rejection of invention patent application after publication