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CN115353130A - Preparation method of defluorination nano magnesium oxide - Google Patents

Preparation method of defluorination nano magnesium oxide Download PDF

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Publication number
CN115353130A
CN115353130A CN202211033157.5A CN202211033157A CN115353130A CN 115353130 A CN115353130 A CN 115353130A CN 202211033157 A CN202211033157 A CN 202211033157A CN 115353130 A CN115353130 A CN 115353130A
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Prior art keywords
fluorine
defluorination
solution
mgcl
magnesium oxide
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Chinese (zh)
Inventor
杨崎峰
朱红祥
雷鸣
林宏飞
郭威
丘能
谭华珊
龙子升
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Guangxi Bossco Environmental Protection Technology Co Ltd
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Guangxi Bossco Environmental Protection Technology Co Ltd
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Priority to CN202211033157.5A priority Critical patent/CN115353130A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/02Magnesia
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • B01J19/0066Stirrers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/041Oxides or hydroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/12Halogens or halogen-containing compounds
    • C02F2101/14Fluorine or fluorine-containing compounds

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Environmental & Geological Engineering (AREA)
  • Hydrology & Water Resources (AREA)
  • Water Supply & Treatment (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Geology (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a preparation method of defluorination nanometer magnesia. In the method, mgCl is added into a constant-temperature stirrer 2 The solution and the dispersing agent are stirred so that MgCl is obtained 2 Mixing the solution and dispersant thoroughly, fixing the constant pressure separating funnel with an iron standAnd pouring a precipitator into the constant-pressure separating funnel, standing the obtained colloid at normal temperature after dropwise adding, washing the colloid twice by using deionized water and absolute ethyl alcohol respectively, transferring the colloid to a tubular furnace filled with nitrogen, calcining the colloid in the tubular furnace, and obtaining the prepared nano magnesium oxide sample after calcining. The nano-magnesia prepared by the method has good crystallinity, the obtained magnesia is uniformly dispersed, and the specific surface area is up to 240m 2 When the fluorine-removing agent is used as a fluorine-removing agent for adsorbing fluorine ions, only 0.5g/L of sample needs to be added into a fluorine ion solution with the concentration of 20ppm, and the effect of fluorine-removing rate of more than 96 percent can be achieved through one-time fluorine removal, so that the fluorine-removing agent is a material with excellent fluorine-removing capability, and the whole preparation process is simple and good in reproducibility.

Description

Preparation method of defluorination nano magnesium oxide
Technical Field
The invention relates to the technical field of nano-magnesia preparation, in particular to a preparation method of defluorination nano-magnesia.
Background
In the existing process technology for preparing the nano magnesium oxide serving as the defluorination material, a hydrothermal method and a sol-gel method are generally used for preparing the nano magnesium oxide, but equipment high-pressure autoclave with certain danger and high cost is required in the hydrothermal process, the sol-gel method preparation process generally needs longer time, the prepared nano magnesium oxide material has serious agglomeration phenomenon, the defluorination capacity of the magnesium oxide is greatly reduced, and the prepared magnesium oxide is limited by precursor materials. Aiming at the problems, the invention regulates the growth speed of the magnesium oxide crystal by regulating the dropping speed of the alkali, and prepares the nano magnesium oxide material with uniform particles, good dispersibility and high specific surface area by a simple mode.
Disclosure of Invention
The invention aims to provide a method for removing fluorineA method for preparing nano magnesium oxide. According to the preparation method of the defluorination nano magnesium oxide, the nano magnesium oxide prepared by the method has good crystallinity, the obtained magnesium oxide is uniformly dispersed, and the specific surface area is as high as 240m 2 When the fluorine removal agent is used as a fluorine removal agent for adsorbing fluorine ions, only 0.5g/L of sample needs to be added into a fluorine ion solution with the concentration of 20ppm, and the effect of fluorine removal rate of more than 96 percent can be achieved through one-time fluorine removal, so that the fluorine removal agent is a material with excellent fluorine removal capability, the whole preparation process is simple, and the reproducibility is good, and the technical scheme adopted by the invention is as follows:
according to one aspect of the invention, the preparation method of the defluorination nanometer magnesia is provided, which comprises the following steps:
(1) Mixing MgCl 2 ·6H 2 Dissolving O in deionized water to prepare MgCl 2 Pouring the solution into a beaker, placing the beaker in a magnetic stirrer at a constant temperature, stirring, adding a dispersing agent, and continuously stirring for 1 hour to obtain MgCl 2 The solution and the dispersant are completely mixed;
(2) Slowly adding a precipitant by using a constant-pressure separating funnel;
(3) After the dropwise addition of the NaOH solution is finished, taking out the beaker filled with the solution, sealing the opening of the beaker by using a preservative film, isolating carbon dioxide in the air, standing for 24 hours at normal temperature, washing by using absolute ethyl alcohol and deionized water until Cl is contained in the washing liquid after washing - Is absent;
(4) And drying the washed white powder in a drying oven at 60 ℃ for 12h, finally calcining in a tubular furnace filled with nitrogen, naturally cooling the tubular furnace after the calcination is finished, and taking out to obtain the prepared nano magnesium oxide sample.
Preferably, mgCl is used in said step (1) 2 The concentration of the solution was 0.25mol/L.
Preferably, the stirring speed in the step (1) is 200rpm, and the stirring temperature is 25 ℃.
Preferably, the dispersant is polyethylene glycol 6000, the proportion of polyethylene glycol 6000 is 3wt% MgCl 2
Preferably, the precipitant in step (2) is a NaOH solution, the concentration of the NaOH solution is 1mol/L, and the NaOH solution is added in a dropwise manner, and the dropwise adding rate is 20 s/drop.
Preferably, the calcination condition in the step (4) is calcination at 500 ℃ for 4h.
The technical scheme adopted by the invention has the following remarkable effects:
MgCl is added into a constant-temperature stirrer 2 The solution and the dispersing agent are stirred so that MgCl is obtained 2 And fully mixing the solution and the dispersing agent, fixing a constant-pressure separating funnel by using an iron support, pouring a precipitator into the constant-pressure separating funnel, standing the obtained colloid at normal temperature after the dropwise addition is finished, washing the colloid twice by using deionized water and absolute ethyl alcohol respectively, transferring the colloid to a tubular furnace filled with nitrogen, and calcining the colloid in the tubular furnace, thus obtaining the prepared nano magnesium oxide sample after calcining and sintering. The nano-magnesia prepared by the method has good crystallinity, the obtained magnesia is uniformly dispersed, and the specific surface area is up to 240m 2 When the fluorine-removing agent is used as a fluorine-removing agent for adsorbing fluorine ions, only 0.5g/L of sample needs to be added into a fluorine ion solution with the concentration of 20ppm, and the effect of fluorine-removing rate of more than 96 percent can be achieved through one-time fluorine removal, so that the fluorine-removing agent is a material with excellent fluorine-removing capability, and the whole preparation process is simple and good in reproducibility.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention;
fig. 2 is a schematic structural diagram of the present invention.
1-constant pressure separating funnel, 2-test tube clamp, 3-magnetic stirrer, 4-beaker, 5-stirring magneton, and 6-test bench.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings by way of examples of preferred embodiments. It should be noted, however, that the numerous details set forth in the description are merely for the purpose of providing the reader with a thorough understanding of one or more aspects of the present invention, which may be practiced without these specific details.
As shown in fig. 1, the preparation method of defluorination nanometer magnesia according to the invention comprises the following steps:
(1) Reacting MgCl 2 ·6H 2 Dissolving O in deionized water to prepare MgCl with the concentration of 0.25mol/L 2 Pouring the solution into a beaker, placing in a constant temperature adding magnetic stirrer, stirring at 200rpm and 25 deg.C for 1 hr, adding dispersant polyethylene glycol 6000 (polyethylene glycol 6000) at a ratio of 3wt% of polyethylene glycol 6000, and adding MgCl 2 Stirring for 1h to obtain MgCl 2 The solution and the dispersant are completely mixed;
(2) Fixing a constant-pressure separating funnel by using an iron support, slowly adding a precipitator which is NaOH solution into the constant-pressure separating funnel, and pouring MgCl according to the molar ratio 2 The dropping speed of NaOH is controlled to be 20 drops/min, the concentration of the NaOH solution is controlled to be 1mol/L, the NaOH solution is added in a dropping mode, and the dropping speed is controlled to be 20 s/drop;
(3) After the dropwise addition of the NaOH solution is finished, taking out the beaker filled with the solution, sealing the opening of the beaker by using a preservative film, isolating carbon dioxide in the air, standing for 24 hours at normal temperature, washing by using absolute ethyl alcohol and deionized water until Cl is contained in the washing liquid after washing - Is absent;
(4) And drying the washed white powder in a drying oven at 60 ℃ for 12h, finally calcining in a tubular furnace filled with nitrogen at 500 ℃ for 4h, naturally cooling the tubular furnace after the calcination is finished, and taking out to obtain the prepared nano magnesium oxide sample.
The nano-magnesia prepared by the method has good crystallinity, the obtained magnesia is uniformly dispersed, the specific surface area is as high as 240m < 2 >/g, when the nano-magnesia is used as a fluorine removal agent for adsorbing fluorine ions, only 0.5g/L of sample needs to be put into a fluorine ion solution with the concentration of 20ppm, and the effect of fluorine removal rate of more than 96 percent can be achieved through one-time fluorine removal, so that the nano-magnesia is a material with excellent fluorine removal capability, and the whole preparation process is simple and has good reproducibility.
As shown in fig. 2, the apparatus used in the present invention includes a constant pressure separatory funnel, the constant pressure separatory funnel is installed in a test tube holder, the test tube holder is installed on a test bench, the constant pressure separatory funnel is filled with sodium hydroxide solution, a magnetic stirrer is arranged below the constant pressure separatory funnel, deionized water is added in the magnetic stirrer, a beaker is arranged in the deionized water, and a mixed solution of magnesium oxide and polyethylene glycol is filled in the beaker.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.

Claims (6)

1. A preparation method of defluorination nanometer magnesia is characterized in that: the method comprises the following steps:
(1) Mixing MgCl 2 ·6H 2 Dissolving O in deionized water to prepare MgCl 2 Pouring the solution into a beaker, placing the beaker in a magnetic stirrer at a constant temperature, stirring, adding a dispersing agent, and continuously stirring for 1 hour to obtain MgCl 2 The solution and the dispersant are completely mixed;
(2) Slowly adding a precipitant by using a constant-pressure separating funnel;
(3) After the dropwise addition of the NaOH solution is finished, taking out the beaker filled with the solution, sealing the opening of the beaker by using a preservative film, isolating carbon dioxide in the air, standing for 24 hours at normal temperature, washing by using absolute ethyl alcohol and deionized water until Cl is contained in the washing liquid after washing - Is absent;
(4) And (3) drying the washed white powder in a drying oven at 60 ℃ for 12 hours, finally calcining in a tubular furnace filled with nitrogen, naturally cooling the tubular furnace after the calcination is finished, and taking out to obtain the prepared nano magnesium oxide sample.
2. The preparation method of the defluorination nanometer magnesia as claimed in claim 1, which is characterized in that: mgCl in the step (1) 2 The concentration of the solution was 0.25mol/L.
3. The preparation method of the defluorination nanometer magnesia as claimed in claim 1, which is characterized in that: the stirring speed in the step (1) is 200rpm, and the stirring temperature is 25 ℃.
4. The method for preparing defluorination nano magnesium oxide according to claim 1, which is characterized in that: the dispersant is polyethylene glycol 6000, the proportion of polyethylene glycol 6000 is 3wt% MgCl 2
5. The preparation method of the defluorination nanometer magnesia as claimed in claim 1, which is characterized in that: and (3) adding the precipitator in the step (2) which is a NaOH solution with the concentration of 1mol/L in a dropwise manner at the dropping rate of 20 s/drop.
6. The method for preparing defluorination nano magnesium oxide according to claim 1, which is characterized in that: the calcining condition in the step (4) is calcining for 4 hours at 500 ℃.
CN202211033157.5A 2022-08-26 2022-08-26 Preparation method of defluorination nano magnesium oxide Pending CN115353130A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101920977A (en) * 2010-08-06 2010-12-22 东北大学 A kind of preparation method of flaky nano magnesium oxide
CN103803591A (en) * 2013-12-27 2014-05-21 厦门大学 Method for preparing ultra-low bulk density magnesium oxide
CN104607142A (en) * 2015-01-20 2015-05-13 中国科学院合肥物质科学研究院 MgO/MgCO3 Composite with Micro-nano Hierarchical Structure and Its Application as Fluoride Removal Agent
CN105366696A (en) * 2015-12-14 2016-03-02 苏州市泽镁新材料科技有限公司 Method for preparing high-purity nanometer magnesia
CN105540623A (en) * 2016-01-14 2016-05-04 华东师范大学 Method for preparing nanometer magnesia
US20210260561A1 (en) * 2020-02-21 2021-08-26 King Fahd University Of Petroleum And Minerals Magnesium oxide-polyamine adsorbent and a method of capturing carbon dioxide

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101920977A (en) * 2010-08-06 2010-12-22 东北大学 A kind of preparation method of flaky nano magnesium oxide
CN103803591A (en) * 2013-12-27 2014-05-21 厦门大学 Method for preparing ultra-low bulk density magnesium oxide
CN104607142A (en) * 2015-01-20 2015-05-13 中国科学院合肥物质科学研究院 MgO/MgCO3 Composite with Micro-nano Hierarchical Structure and Its Application as Fluoride Removal Agent
CN105366696A (en) * 2015-12-14 2016-03-02 苏州市泽镁新材料科技有限公司 Method for preparing high-purity nanometer magnesia
CN105540623A (en) * 2016-01-14 2016-05-04 华东师范大学 Method for preparing nanometer magnesia
US20210260561A1 (en) * 2020-02-21 2021-08-26 King Fahd University Of Petroleum And Minerals Magnesium oxide-polyamine adsorbent and a method of capturing carbon dioxide

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
朱志彪: ""MgO超细粉体的制备与表征"", 《黑龙江大学自然科学学报》, no. 01, pages 110 - 113 *

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Application publication date: 20221118

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