CN114733269B - Method for cleaning titanium gypsum filter cloth - Google Patents

Method for cleaning titanium gypsum filter cloth Download PDF

Info

Publication number
CN114733269B
CN114733269B CN202210456247.9A CN202210456247A CN114733269B CN 114733269 B CN114733269 B CN 114733269B CN 202210456247 A CN202210456247 A CN 202210456247A CN 114733269 B CN114733269 B CN 114733269B
Authority
CN
China
Prior art keywords
filter cloth
titanium gypsum
soluble
fluoride
soaking
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.)
Active
Application number
CN202210456247.9A
Other languages
Chinese (zh)
Other versions
CN114733269A (en
Inventor
李丽娜
豆君
席岩星
王嘉雍
张玉荣
陈建立
贺高峰
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.)
Longbai Group Co ltd
Original Assignee
Longbai Group Co ltd
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 Longbai Group Co ltd filed Critical Longbai Group Co ltd
Priority to CN202210456247.9A priority Critical patent/CN114733269B/en
Publication of CN114733269A publication Critical patent/CN114733269A/en
Application granted granted Critical
Publication of CN114733269B publication Critical patent/CN114733269B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D41/00Regeneration of the filtering material or filter elements outside the filter for liquid or gaseous fluids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D25/00Filters formed by clamping together several filtering elements or parts of such elements
    • B01D25/32Removal of the filter cakes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Filtering Materials (AREA)

Abstract

The application discloses a method for cleaning titanium gypsum filter cloth, which at least comprises the following steps: s1, removing titanium gypsum on the surface of titanium gypsum filter cloth, and soaking the filter cloth with acid liquor with the acidity of 1-4 mol/L to remove acid-soluble impurities; s2, soaking the filter cloth by adopting a soluble fluoride salt solution; s3, soaking the filter cloth by adopting an iron source solution and/or an aluminum source solution, and then washing to obtain the clean filter cloth. Compared with the prior art, the method has the advantages that acid liquor is firstly adopted to soak and remove acid-soluble impurities such as ferric hydroxide and the like remained in the filter cloth, then soluble fluoride salt is adopted to convert calcium sulfate in the filter cloth into calcium fluoride, then the calcium fluoride reacts with an iron source and/or an aluminum source to generate a water-soluble hexafluoro metal complex and a water-soluble calcium salt, and the water flux of the filter cloth is completely recovered through washing and separation of the filter cloth, so that the purpose of repeatedly using the filter cloth is realized.

Description

Method for cleaning titanium gypsum filter cloth
Technical Field
The invention belongs to the technical field of titanium dioxide production, and particularly relates to a method for cleaning titanium gypsum filter cloth.
Background
In the production process of titanium dioxide by the sulfuric acid method, a large amount of acid wastewater with sulfuric acid as a main component is generated. At present, carbide sludge is often adopted to neutralize the acid wastewater in the treatment process. After the neutralization reaction, a large amount of titanium gypsum with calcium sulfate as the main component is produced. In the filter pressing process, as calcium sulfate crystals continuously grow, not only are filter cloth easy to block and harden, but also the filter cloth cannot be reused completely due to the problems of difficult cleaning and the like, so that the utilization rate of the filter cloth is reduced.
Disclosure of Invention
The invention aims to provide a method for cleaning titanium gypsum filter cloth to solve the defects in the prior art.
The invention aims at realizing the following technical scheme:
a method of cleaning titanium gypsum filter cloth, comprising at least the steps of:
s1, removing titanium gypsum on the surface of titanium gypsum filter cloth, and soaking the filter cloth with acid liquor with the acidity of 1-4 mol/L to remove acid-soluble impurities;
s2, soaking the filter cloth by adopting a soluble fluoride salt solution, and converting slightly soluble calcium sulfate in the filter cloth into insoluble calcium fluoride and water-soluble sulfate;
s3, soaking the filter cloth by adopting an iron source solution and/or an aluminum source solution, converting the insoluble calcium fluoride into a water-soluble hexafluoro metal complex and a water-soluble calcium salt, and then washing to remove the water-soluble hexafluoro metal complex and the water-soluble calcium salt to obtain the clean filter cloth.
Preferably, the acid liquor in the step S1 is recycled until the pH value is more than or equal to 1.
Preferably, the acid solution in step S1 is hydrochloric acid or nitric acid solution.
Preferably, the soaking time in the step S1 is 1.5-2.5 hours.
Preferably, the fluoride salt solution concentration in step S2 is > 50mg/L calculated as fluoride ion.
Preferably, the soaking time in the step S2 is more than or equal to 2 hours, and the temperature of the fluoride salt solution is less than or equal to 60 ℃.
Preferably, the fluoride salt is one or more selected from sodium fluoride and potassium fluoride.
Preferably, the iron source in step S3 is one or more combinations selected from ferric chloride and ferric nitrate, and the aluminum source is one or more combinations selected from aluminum chloride and aluminum nitrate.
Preferably, the filter cloth is soaked by adopting an aluminum source solution, the concentration of the aluminum source solution is more than or equal to 0.7mol/L, and the soaking time is 1.5-2.5 h.
Preferably, the filter cloth is soaked by adopting an iron source solution, the concentration of the iron source solution is more than or equal to 0.7mol/L, and the soaking time is 1.5-2.5 h.
Compared with the prior art, the method has the advantages that acid liquor is firstly adopted to soak and remove acid-soluble impurities such as ferric hydroxide and the like remained in the filter cloth, then soluble fluoride salt is adopted to convert calcium sulfate in the filter cloth into calcium fluoride, then the calcium fluoride reacts with an iron source and/or an aluminum source to generate a water-soluble hexafluoro metal complex and a water-soluble calcium salt, and the water flux of the filter cloth is completely recovered through washing and separation of the filter cloth, so that the purpose of repeatedly using the filter cloth is realized.
Detailed Description
A method of cleaning titanium gypsum filter cloth, comprising the steps of:
s1, removing titanium gypsum on the surface of titanium gypsum filter cloth, then placing the filter cloth in 1-4 mol/L acid liquor for soaking, wherein calcium sulfate is removed from the filter cloth, hydroxide such as ferric hydroxide generated in the neutralization process is also contained in the filter cloth, and the hydroxide is dissolved in acid through acid liquor soaking and can be removed from the calcium sulfate through washing;
s2, soaking the filter cloth by adopting a soluble fluoride salt solution, and converting the slightly soluble calcium sulfate crystals in the filter cloth into insoluble calcium fluoride and water-soluble sulfate; because the solubility of the calcium fluoride is low, the calcium sulfate in the filter cloth can be completely converted into the calcium fluoride; the fluoride salt is required to be fluoride salt which reacts with sulfate radical to generate soluble sulfate solution, such as sodium fluoride and potassium fluoride;
s3, soaking the filter cloth by adopting an iron source solution and/or an aluminum source solution, and reacting the insoluble calcium fluoride with the iron source or the aluminum source to convert into a water-soluble complex ([ FeF) 6 ] 3- Or [ AlF ] 6 ] 3- ) And a water-soluble calcium salt, and then removed from the filter cloth by washing to obtain a clean filter cloth which can be reused. The iron source or aluminum source is required to be used for generating soluble calcium salt solution by reacting with calcium ions, such as ferric chloride and aluminum chloride.
Therefore, the method firstly adopts acid liquor to soak and remove acid-soluble impurities such as ferric hydroxide and the like remained in the filter cloth, then adopts soluble fluoride salt to convert calcium sulfate in the filter cloth into calcium fluoride, then reacts with an iron source and/or an aluminum source to generate a water-soluble hexafluoro metal complex and a water-soluble calcium salt, and the water flux of the filter cloth is basically and completely recovered through washing and separation of the filter cloth, so that the purpose of repeatedly using the filter cloth is realized.
Preferably, the acid liquor in the step S1 is recycled until the pH value is more than or equal to 1 and the recycling is stopped when the acidity is weakened.
Preferably, the acid solution in step S1 can be nitric acid or hydrochloric acid solution.
Preferably, the soaking time in the step S1 is 1.5-2.5 hours, and in this range, acid-soluble impurities can be sufficiently removed.
Preferably, the concentration of the fluoride salt solution in the step S2 is more than 50mg/L in terms of fluoride ion, and saturated fluoride salt solution can be adopted when the fluoride salt solution is used for the first time, and when the concentration of the fluoride salt solution is reduced to be less than or equal to 50mg/L, the fluoride salt solution stops recycling, so that incomplete reaction with calcium sulfate due to lower fluoride salt content is prevented.
Preferably, the soaking time in the step S2 is not less than 2 hours, the fluoride salt solution can be heated to accelerate the reaction, and the heating temperature is less than or equal to 60 ℃.
Preferably, the iron source in the step S3 is one or more combinations selected from ferric chloride and ferric nitrate, and the aluminum source is one or more combinations selected from aluminum chloride and aluminum nitrate.
Preferably, the filter cloth is soaked by adopting an aluminum source solution, the concentration of the aluminum source solution is more than or equal to 0.7mol/l, and the soaking time is 1.5-2.5 h.
Preferably, the filter cloth is soaked by adopting an iron source solution, the concentration of the iron source solution is more than or equal to 0.7mol/l, and the soaking time is 1.5-2.5 h.
Example 1
1. After the titanium gypsum is removed from the plate, the surface of the filter cloth is washed by an external water pipe to remove the incompletely removed titanium gypsum, the filter cloth is removed, the flux of the filter cloth is about 20 percent of that of the fresh filter cloth, and the calcium sulfate content in the filter cloth is 2.3Kg/m 2 (on a calcium sulfate dihydrate dry basis);
2. soaking the filter cloth by using acid liquor (preferably, submerging the filter cloth), wherein the acid liquor is hydrochloric acid, the concentration of the hydrochloric acid is 2mol/L, the soaking time is 2 hours, and then washing by using clear water;
3. soaking the filter cloth by using a hot sodium fluoride solution, wherein the temperature of the solution is 45 ℃, the sodium fluoride content is 9.4g/L (calculated by fluoride ions), the soaking time is 2 hours, and washing by using clear water;
4. soaking the filter cloth by using aluminum chloride, wherein the concentration of the aluminum chloride solution is 0.92mol/l, and the soaking time is 2 hours;
5. then the filter cloth is washed by primary water, the flux of the filter cloth is about 80 percent of that of the fresh filter cloth, and the calcium sulfate content in the filter cloth is 0.45Kg/m 2 The filter cloth (based on the dry basis of calcium sulphate dihydrate) is reusable.
Example 2
1. After the titanium gypsum is removed from the plate, the surface of the filter cloth is washed by an external water pipe to remove the incompletely removed titanium gypsum, the filter cloth is removed, the flux of the filter cloth is about 38% of that of fresh filter cloth, and the content of crystalline calcium sulfate in the filter cloth is 1.51Kg/m 2 (on a calcium sulfate dihydrate dry basis);
2. soaking the filter cloth by using acid liquor (preferably, submerging the filter cloth), wherein the acid liquor is hydrochloric acid, the concentration of the hydrochloric acid is 1.3mol/L, the soaking time is 2 hours, and then washing by using clear water;
3. soaking the filter cloth by using a hot sodium fluoride solution, wherein the temperature of the solution is 36 ℃, the sodium fluoride content is 2.6g/L (calculated by fluoride ions), the soaking time is 2 hours, and washing by using clear water;
4. soaking the filter cloth by using aluminum chloride, wherein the concentration of the aluminum chloride is 1.35mol/l, and the soaking time is 2 hours;
5. the filter cloth was then washed with primary water, at which time the filter cloth flux was about 69% of the fresh filter cloth, and the crystalline calcium sulfate content of the filter cloth was 0.81Kg/m 2 The filter cloth (based on the dry basis of calcium sulphate dihydrate) is reusable.
Comparative example 1
1. After the titanium gypsum is unloaded, the surface of the filter cloth is washed by an external water pipe to remove the incompletely unloaded titanium gypsum;
2. soaking the filter cloth by using acid liquor, wherein the acid liquor is hydrochloric acid, the acidity is 3mol/L, the soaking time is 4 hours, and washing is performed by using clear water;
3. the filter cloth is still in a hardened state and cannot be used.
Comparative example 2
1. After the titanium gypsum is unloaded, the surface of the filter cloth is washed by an external water pipe to remove the incompletely unloaded titanium gypsum;
2. soaking the filter cloth by using sodium hydroxide solution, wherein the alkalinity of the sodium hydroxide solution is 2mol/L, the soaking time is 2h, and washing by using clear water;
3. the filter cloth is still not hardened and cannot be used.
Comparative example 3
1. After the titanium gypsum is unloaded, the surface of the filter cloth is washed by an external water pipe to remove the incompletely unloaded titanium gypsum;
2. soaking the filter cloth by using acid liquor, wherein the acid liquor is hydrochloric acid, the acidity is 3mol/L, the soaking time is 4 hours, and washing is performed by using clear water;
3. soaking the filter cloth by using sodium carbonate solution for 4 hours, and washing by using clear water;
4. the filter cloth is soaked by acid liquor, the acid liquor is hydrochloric acid, the acid is 3mol/L, the soaking time is 4 hours, and a large number of bubbles are generated due to the reaction, so that the determination of the reaction end point is difficult and cannot be conveniently determined.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention. It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.

Claims (10)

1. A method of cleaning titanium gypsum filter cloth, comprising at least the steps of:
s1, removing titanium gypsum on the surface of titanium gypsum filter cloth, and soaking the filter cloth with acid liquor with the acidity of 1-4 mol/L to remove acid-soluble impurities;
s2, soaking the filter cloth by adopting a soluble fluoride salt solution, and converting slightly soluble calcium sulfate in the filter cloth into insoluble calcium fluoride and water-soluble sulfate;
s3, soaking the filter cloth by adopting an iron source solution and/or an aluminum source solution, converting the insoluble calcium fluoride into a water-soluble hexafluoro metal complex and a water-soluble calcium salt, and then washing to remove the water-soluble hexafluoro metal complex and the water-soluble calcium salt to obtain the clean filter cloth.
2. A method of cleaning titanium gypsum filter cloth according to claim 1,
and (3) recycling the acid liquor in the step (S1) until the pH value is more than or equal to 1.
3. A method of cleaning titanium gypsum filter cloth according to claim 1,
the acid liquid in the step S1 is hydrochloric acid or nitric acid solution.
4. A method of cleaning titanium gypsum filter cloth according to claim 1,
the soaking time in the step S1 is 1.5-2.5 h.
5. A method of cleaning titanium gypsum filter cloth according to claim 1,
the concentration of the fluoride salt solution in the step S2 is calculated by fluoride ion, and the concentration is more than 50mg/L.
6. A method of cleaning titanium gypsum filter cloth according to claim 1,
the soaking time in the step S2 is more than or equal to 2 hours, and the temperature of the fluoride salt solution is less than or equal to 60 ℃.
7. A method of cleaning titanium gypsum filter cloth according to claim 1,
the fluoride salt is one or more selected from sodium fluoride and potassium fluoride.
8. A method of cleaning titanium gypsum filter cloth according to claim 1,
the iron source in the step S3 is one or more combinations selected from ferric chloride and ferric nitrate, and the aluminum source is one or more combinations selected from aluminum chloride and aluminum nitrate.
9. A method of cleaning titanium gypsum filter cloth according to claim 8,
the filter cloth is soaked by adopting an aluminum source solution, the concentration of the aluminum source solution is more than or equal to 0.7mol/L, and the soaking time is 1.5-2.5 h.
10. A method of cleaning titanium gypsum filter cloth according to claim 8,
the filter cloth is soaked by adopting an iron source solution, the concentration of the iron source solution is more than or equal to 0.7mol/L, and the soaking time is 1.5-2.5 h.
CN202210456247.9A 2022-04-28 2022-04-28 Method for cleaning titanium gypsum filter cloth Active CN114733269B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210456247.9A CN114733269B (en) 2022-04-28 2022-04-28 Method for cleaning titanium gypsum filter cloth

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210456247.9A CN114733269B (en) 2022-04-28 2022-04-28 Method for cleaning titanium gypsum filter cloth

Publications (2)

Publication Number Publication Date
CN114733269A CN114733269A (en) 2022-07-12
CN114733269B true CN114733269B (en) 2024-02-06

Family

ID=82282806

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210456247.9A Active CN114733269B (en) 2022-04-28 2022-04-28 Method for cleaning titanium gypsum filter cloth

Country Status (1)

Country Link
CN (1) CN114733269B (en)

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB885383A (en) * 1958-01-17 1961-12-28 Gen Am Transport Recovery of depleted chemical nickle plating baths
US4139465A (en) * 1976-11-26 1979-02-13 Nordengren Patenter Ab Method for washing filter-cakes and a spray nozzle intended for use with the method
US4159308A (en) * 1975-06-30 1979-06-26 The University Of Melbourne Mineral treatment
SU1342285A1 (en) * 1986-02-25 1995-07-09 Всесоюзный Государственный Научно-Исследовательский И Проектный Институт Химико-Фотографической Промышленности Method of chemical-photographic treatment of halogen-silver photographic materials
JPH10137744A (en) * 1996-11-11 1998-05-26 Nec Corp Treatment of waste water containing fluorine
WO2002004361A1 (en) * 2000-07-07 2002-01-17 Microbar, Inc. System and method for simultaneous removal of arsenic and fluoride from aqueous solutions
CN101658746A (en) * 2009-09-16 2010-03-03 朱峰 Method for removing crystallization scales on plastic film filter plate of electroplating wastewater
CN108360070A (en) * 2018-01-19 2018-08-03 西安建筑科技大学 A kind of normal temperature modified method improving hemihydrate calcium sulfate crystal whisker stability
CN108373140A (en) * 2018-02-26 2018-08-07 中南大学 A method of removing fluorine from sulfate liquor
CN212166735U (en) * 2019-11-27 2020-12-18 常州广威新材料科技有限公司 Belt filter cloth belt cleaning device is used in calcium sulfate whisker production

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB885383A (en) * 1958-01-17 1961-12-28 Gen Am Transport Recovery of depleted chemical nickle plating baths
US4159308A (en) * 1975-06-30 1979-06-26 The University Of Melbourne Mineral treatment
US4139465A (en) * 1976-11-26 1979-02-13 Nordengren Patenter Ab Method for washing filter-cakes and a spray nozzle intended for use with the method
SU1342285A1 (en) * 1986-02-25 1995-07-09 Всесоюзный Государственный Научно-Исследовательский И Проектный Институт Химико-Фотографической Промышленности Method of chemical-photographic treatment of halogen-silver photographic materials
JPH10137744A (en) * 1996-11-11 1998-05-26 Nec Corp Treatment of waste water containing fluorine
WO2002004361A1 (en) * 2000-07-07 2002-01-17 Microbar, Inc. System and method for simultaneous removal of arsenic and fluoride from aqueous solutions
CN101658746A (en) * 2009-09-16 2010-03-03 朱峰 Method for removing crystallization scales on plastic film filter plate of electroplating wastewater
CN108360070A (en) * 2018-01-19 2018-08-03 西安建筑科技大学 A kind of normal temperature modified method improving hemihydrate calcium sulfate crystal whisker stability
CN108373140A (en) * 2018-02-26 2018-08-07 中南大学 A method of removing fluorine from sulfate liquor
CN212166735U (en) * 2019-11-27 2020-12-18 常州广威新材料科技有限公司 Belt filter cloth belt cleaning device is used in calcium sulfate whisker production

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Removal of F −and organic matter from coking wastewater by coupling dosing FeCl 3 and AlCl 3;Shuo Li等;《Journal of environmental sciences》 *

Also Published As

Publication number Publication date
CN114733269A (en) 2022-07-12

Similar Documents

Publication Publication Date Title
CN100532268C (en) Production method of oxygen-containing beta aluminum fluoride for aluminum electrolysis bath by using aluminum scruff ash
CN104071820A (en) Method for producing calcium fluoride by waste LCD panel glass etching liquid
JP6288217B1 (en) Method and apparatus for treating wastewater containing sulfuric acid, fluorine and heavy metal ions
IE832401L (en) Polishing glass articles in an acid bath
CN114524572B (en) Comprehensive treatment method for wastewater generated in iron phosphate production
CN114733269B (en) Method for cleaning titanium gypsum filter cloth
CN110902883A (en) Recycling method of fluorine-containing wastewater
CN112456443B (en) Recovery processing method and recovery processing device for glass etching waste liquid
US20090145856A1 (en) Acid recycle process with iron removal
US4044106A (en) Reclamation of phosphate from bright dip drag-out
CN104803522B (en) A kind of processing method of high sodium fluoride waste
CN108341514B (en) Method for treating wastewater generated in purification process by using graphite acid method
CN108950581B (en) Regeneration method of stainless steel mixed pickling waste acid
CN115283422A (en) Treatment method of glass etching waste residue
CN114715904A (en) Method for cooperatively treating CVD dust and ammonium chloride waste liquid
CN114906957A (en) Concentrated brine recycling treatment method and treatment system
JP2912934B2 (en) Method for treating wastewater containing borofluoride ions
CN108914136B (en) Steel pipe galvanizing pretreatment process
KR100691165B1 (en) Method for recovering of h2so4 produced in pickling process
JP2005144209A (en) Fluorine-containing waste water treatment method
CN108164071B (en) Method for recovering bromine salt from flue gas absorption liquid
CN113213549A (en) Method for producing polymeric ferric sulfate by recycling waste acid
US5022971A (en) Process for the electrolytic pickling of high-grade steel strip
CN111470661A (en) Method for recovering and preparing aluminum-containing compound and sulfite from aluminum-containing waste alkali liquor
CN111634936A (en) Method for producing praseodymium neodymium fluoride by using fluorine-containing wastewater

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
GR01 Patent grant
GR01 Patent grant