CN108439441A - A kind of method of normal pressure short route production magnesium hydroxide - Google Patents
A kind of method of normal pressure short route production magnesium hydroxide Download PDFInfo
- Publication number
- CN108439441A CN108439441A CN201810203171.2A CN201810203171A CN108439441A CN 108439441 A CN108439441 A CN 108439441A CN 201810203171 A CN201810203171 A CN 201810203171A CN 108439441 A CN108439441 A CN 108439441A
- Authority
- CN
- China
- Prior art keywords
- magnesium
- magnesium hydroxide
- mgcl
- normal pressure
- brine
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A kind of method of normal pressure short route production magnesium hydroxide, is that will first contain magnesium material stirring to be added in ammonium chloride solution, makes its decomposition, adjust pH purification and impurity removals, refined brine is filtered to obtain, alkaline matter tune pH is then added into gained brine makes magnesium precipitate therein be precipitated, and filters to obtain Mg (OH)2Liquid after filter cake and magnesium sinking；Gained Mg (OH)2Filter cake MgCl2Solution heating transition, is filtered, washed, dries to obtain crystal form magnesium hydroxide products；Liquid stirring is passed through by CO after magnesium sinking2With NH3The mixed gas Precipitation calcium therein of composition, filters to obtain liquid after winnofil and heavy calcium, and gained sinks liquid return after calcium and continues on for material containing magnesium and decompose.The present invention have it is simple for process, easy to operate, reagent consumption is few, and processing cost is low, good product quality, no waste water, exhaust gas discharge, Primary Chemical can closed cycle use the advantages that, be suitable for the magnesium hydroxide industrialized production of material production containing magnesium application.
Description
Technical field
The invention belongs to chemical industry and field of metallurgy, and in particular to a kind of method of normal pressure short route production magnesium hydroxide.
Background technology
Magnesium hydroxide is colourless hexagonal prism crystal or white powder, is insoluble in water and alcohol, is dissolved in diluted acid and ammonium salt solution, water
Solution is in alkalescent.Magnesium hydroxide is heated to 350 DEG C and loses water generation magnesia.Magnesium hydroxide be added to polyethylene, polypropylene,
In polystyrene and ABS resin, there is good fire-retardant and smoke elimination effect, be a kind of novel filled-type fire retardant.Magnesium hydroxide is logical
It crosses and is released when being thermally decomposed in conjunction with water, absorb a large amount of latent heat, to reduce the table of synthetic material that it is filled in flame
Face temperature has the function of that polymer is inhibited to decompose and carry out cooling to generated fuel gas.Decompose the magnesia generated
It is good refractory material again, can also helps the fire resistance for improving synthetic material, while the vapor that it is released also can be used as
A kind of smoke suppressant.Magnesium hydroxide is that have fire-retardant, suppression cigarette, the outstanding fire retardant for filling triple functions in generally acknowledged rubber and plastic industry.
It is widely used in the high molecular materials such as rubber, chemical industry, building materials, plastics and electronics, unsaturated polyester (UP) and paint, coating.
The industrial process of magnesium hydroxide mainly has brine --- lime method and dolomite acid hydrolyzation.Brine --- lime method
It is that brine is added in milk of lime (to contain MgCl2Solution) in Precipitation Mg (OH)2, sediment is washed again, settle, be separated by filtration,
Dry, crushing, obtains magnesium hydroxide products.Dolomite acid hydrolyzation is divided into hydrochloric acid method and sulfuric acid process.Hydrochloric acid method is decomposed with hydrochloric acid
Dolomite and its high temperature pyrolysis product must contain MgCl2Brine, gained brine adds milk of lime or ammonia precipitation process that Mg (OH) is precipitated2, sink
Starch is washed again, settles, is separated by filtration, drying, crushing, and obtains magnesium hydroxide products.Sulfuric acid process is to use sulfuric acid decomposition white clouds
Stone and its high temperature pyrolysis product obtain Adlerika, gained Adlerika ammonification Precipitation Mg (OH)2, sediment is again through washing
It washs, settle, be separated by filtration, dry, crush, obtain magnesium hydroxide products.Containing MgCl2The direct neutralization precipitation of brine be precipitated be
Cotton-shaped Mg (OH)2Sediment will improve its strainability, need (24-48h) ageing for a long time that can just be converted to crystalline precipitation.
Therefore, crystal form magnesium hydroxide is prepared at present and mostly use hydrothermal synthesis method greatly, i.e., first by MgCl2Mg is precipitated in solution neutralization precipitation
(OH)2, then sediment is transferred in autoclave, it is allowed to convert through 140-180 DEG C (pressure 0.36-1.02MPa) processing 4-8h
At crystal Mg (OH)2Afterwards, refilter, wash, drying and to obtain crystal form magnesium hydroxide products.It is therefore seen that these magnesium hydroxides produce
Technique, not only technological process is long, high energy consumption, and reagent consumption is big, and the waste water of generation is more, seriously polluted.
Invention content
The purpose of the present invention is to provide a kind of good product qualities, and processing cost is low, easy to operate, and environmental-friendly contains magnesium
The method of material production magnesium hydroxide.
A kind of method of normal pressure short route production magnesium hydroxide of the present invention, is toward containing MgCl2Brine in be passed through ammonia or
Lime is added, adjusts pH value of solution to 9.5-12.5, so that magnesium precipitate therein is precipitated, solid-liquor separation obtains Mg (OH)2Sediment and heavy
Then liquid after magnesium presses liquid-solid ratio 1:0.5-5g/mL is by gained Mg (OH)2Sediment is added to the MgCl of a concentration of >=1.5mol/L2
In solution, 105-185 DEG C of transition is filtered, washed, dries to obtain crystal form magnesium hydroxide products.
A kind of method of normal pressure short route production magnesium hydroxide of the present invention, magnesium hydrate precipitate precipitation process, control system
Temperature is at 20-90 DEG C, reaction time 0.5-5.5h.
A kind of method of normal pressure short route production magnesium hydroxide of the present invention, MgCl2Solution concentration is 1.5-7.5mol/L, is turned
Type time 1-8h.
A kind of method of normal pressure short route production magnesium hydroxide of the present invention, contains MgCl2Brine using following techniques prepare：
Magnesium material will be contained and be added to NH4In Cl solution, 150 DEG C of reactions stirred below filter to contain MgCl2Brine, reaction
The gas collection reuse of generation；
The addition of the material containing magnesium is converted to MgCl by the magnesium in material containing magnesium21-3 times of theoretical amount determine, NH4Cl solution
A concentration of 1.5-15mol/L, mix thoroughly reaction temperature be 0-150 DEG C, reaction time 0.5-5.5h；
The material containing magnesium is selected from magnesite stone ore (MgCO3), dolomite mineral (CaMg (CO3)2) and its high temperature thermal decomposition product
At least one of.
In the present invention, the gas collection reuse refers to that the gas for generating reaction is introduced directly into containing MgCl2Brine or
After refined brine or magnesium sinking in liquid, or through lime removing CO therein2It is imported again containing MgCl afterwards2Brine or refined brine or heavy
After magnesium in liquid, it is allowed to be converted to NH4Cl, or be allowed to be converted to NH with hydrochloric acid or calcium chloride solution absorption4Cl is recycled in process to be made
With.
A kind of method of normal pressure short route production magnesium hydroxide of the present invention, contains MgCl2Making from brine it is standby during,
It is stirred to react when rising to 4.5-9.4 to pH value of solution, oxidizing agent scavenging removal of impurities is added, filter to contain MgCl2Essence
Brewed brine water；The oxidant is selected from least one of hydrogen peroxide, calcium hypochlorite, magnesium hypochlorite, chlorine.
In the present invention, the pH value of solution rising refers to material containing magnesium and NH4Cl reaction process, pH value of solution rise to naturally
4.5-9.4, or alkaline matter is added in reaction solution, so that its pH is risen to 4.5-9.4；The alkaline matter is selected from ammonia
Gas, ammonium hydroxide, lime, magnesia, magnesium hydroxide, at least one of calcium hypochlorite, magnesium hypochlorite.
A kind of method of normal pressure short route production magnesium hydroxide of the present invention, CO is passed through into liquid after the magnesium sinking2Gas, and
Adjust pH value of solution to 3.5-8.5 with ammonia, 0~60 DEG C of 0.5~6.5h of reaction, filter calcium carbonate filter cake and regeneration ammonium chloride it is molten
Liquid, gained, which regenerates ammonium chloride solution and returns, contains MgCl2Brine preparation section recycle.
The basic principle of the magnesium hydroxide of material production containing magnesium can be indicated with following formulas：
MgCO3+2NH4Cl=Δs=MgCl2+CO2↑+2NH3↑+H2O (1)
CaMg(CO3)2+4NH4Cl=Δs=CaCl2+MgCl2+2CO2↑+4NH3↑+2H2O (2)
CaO+2NH4Cl=CaCl2+H2O+2NH3↑ (3)
MgO+2NH4Cl=MgCl2+H2O+2NH3↑ (4)
CaO+CO2=CaCO3 (5)
Ca(OH)2+CO2=CaCO3+H2O (6)
MgCl2+H2O+2NH3=2NH4Cl+Mg(OH)2↓ (7)
MgCl2+Ca(OH)2=CaCl2+Mg(OH)2↓ (8)
CaCl2+H2O+2NH3+CO2=2NH4Cl+CaCO3↓ (8)
The present invention is had the following advantages compared with existing technology and effect：
Present invention NH4Cl solution decomposes material containing magnesium, effectively inhibits the dissolution of impurity F e, Al, Si etc., is contained
MgCl2Brine, significantly reduce solution purification removal of impurities burden, and utilize NH4Cl and NH3Mutual conversion, will dexterously contain
Magnesium in magnesium material is separated and recovered with calcium, realizes NH4Cl is recycled technical process；Utilize MgCl2The boiling point of solution is with it
The increase of concentration and the characteristics of increase, with containing MgCl2Solution thermal precipitation be precipitated Mg (OH)2, it is allowed under normal pressure through 105-
185 DEG C are converted to crystal form magnesium hydroxide, and traditional handicraft is needed Mg (OH)2Sediment can just obtain crystalline substance through high temperature high pressure process
Type magnesium hydroxide products, have it is simple for process, easy to operate, reagent consumption is few, and processing cost is low, good product quality, no waste water,
Exhaust gas discharge, Primary Chemical can closed cycle use the advantages that, be suitable for magnesium hydroxide industrialized production application.
Specific implementation mode
With reference to embodiment, the invention will be further described, following embodiment be intended to illustrate invention rather than it is right
The present invention's further limits.
Embodiment 1
The ammonium chloride solution 2.5L of 9mol/L, 105 DEG C of stirrings is taken to be slowly added to the dolomite miberal powder of -250 mesh, wait for solution
After pH rises to 4.5, appropriate hydrogen peroxide is added and continues to stir 0.5h, removes the impurity such as aluminium, iron, the manganese in solution, filters to contain
CaCl2And MgCl2Refined brine.It reacts the gas generated and recycles NH with calcium chloride solution spray-absorption4Cl.Then toward gained
Stirring adds Ca (OH) in refined brine2PH to 12.5 is adjusted, precipitation magnesium hydroxide is staticly settled, filters to obtain (OH) containing Mg2Filter
Liquid after cake and magnesium sinking；Gained (OH) containing Mg2Filter cake press solid-to-liquid ratio 1:1.5g/ml is added to the MgCl of 6.5mol/L2In solution,
135 DEG C of stirring transition 2.5h are filtered, washed, dry to obtain nanocrystal magnesium hydroxide products of the purity up to 99.3%.Finally, exist
Stirring is passed through by CO in liquid after magnesium sinking2With NH3The mixed gas Precipitation calcium therein of composition, filter purity up to 99.6%
Lightweight CaCO3And its liquid after precipitation.
Embodiment 2
Magnesite miberal powder of -180 purposes containing dolomite is slowly added to after the precipitation of calcium carbonate that embodiment 1 obtains in liquid,
Calcium hypochlorite tune pH to 5.1 is added after pH value of solution rises to 3.8 in 110 DEG C of stirrings, continues to stir 0.5h, filters to obtain refined halogen
Water.It reacts the gas generated and recycles ammonium chloride with absorption by Hydrochloric Acid.Then it refines stirring in brine toward gained and is passed through ammonia tune pH extremely
12.2, Precipitation magnesium hydroxide filters to obtain Mg (OH)2Liquid after filter cake and magnesium sinking；Gained Mg (OH)2Filter cake presses solid-to-liquid ratio 1:2g/
Ml is added to the MgCl of 5.5mol/L2In solution, 125 DEG C of stirring transition 4.5h, be filtered, washed, dry purity up to 99.6%
Nanocrystal magnesium hydroxide products.Finally, stirring is passed through by CO in liquid after magnesium sinking2With NH3The mixed gas precipitation analysis of composition
Go out calcium therein, filters to obtain CaCO of the purity up to 99.4%3And its liquid after precipitation.
Embodiment 3
Prepare the ammonium chloride solution 5m of 12mol/L3, 15 DEG C are stirred addition dolomite mineral calcining and decomposing products, wait for pH value of solution
7.2 are risen to, magnesium hypochlorite tune pH to 7.4 is added, continues to stir 1h, filters to obtain refined brine, then refined in brine toward gained,
120 DEG C of stirrings are slowly added to light calcined magnesia, wait for that pH value of solution rises to 10.8, stop charging, lead to ammonia tune pH to 11.8, continue to stir
4h is filtered, washed, dries to obtain nanocrystal magnesium hydroxide products of the purity up to 98.1%.Finally, it is stirred into gained filtrate logical
Enter by CO2With NH3The mixed gas Precipitation calcium therein of composition filters to obtain CaCO of the purity up to 99.2%3And its after precipitation
Liquid.
Claims (10)
1. a kind of method of normal pressure short route production magnesium hydroxide, is toward containing MgCl2Brine in be passed through ammonia or be added lime,
PH value of solution is adjusted to 9.5-12.5, so that magnesium precipitate therein is precipitated, solid-liquor separation obtains Mg (OH)2Liquid after sediment and magnesium sinking, so
Liquid-solid ratio 1 is pressed afterwards:0.5-5g/mL is by gained Mg (OH)2Sediment is added to the MgCl of a concentration of >=1.5mol/L2In solution,
105-185 DEG C of transition, is filtered, washed, dries to obtain crystal form magnesium hydroxide products.
2. a kind of method of normal pressure short route production magnesium hydroxide according to claim 1, it is characterised in that：Magnesium hydroxide
Precipitation process, control system temperature is at 20-90 DEG C, reaction time 0.5-5.5h.
3. a kind of method of normal pressure short route production magnesium hydroxide according to claim 1, it is characterised in that：MgCl2Solution
A concentration of 1.5-7.5mol/L, make the transition time 1-8h.
4. a kind of method of normal pressure short route production magnesium hydroxide according to claim 1, contains MgCl2Brine use under
State technique preparation：
Magnesium material will be contained and be added to NH4In Cl solution, 150 DEG C of reactions stirred below filter to contain MgCl2Brine, reaction generate
Gas collection reuse.
5. a kind of method of normal pressure short route production magnesium hydroxide according to claim 4, it is characterised in that：It is described to contain magnesium
Material is selected from magnesite stone ore (MgCO3), dolomite mineral (CaMg (CO3)2At least one of) and its high temperature thermal decomposition product.
6. a kind of method of normal pressure short route production magnesium hydroxide according to claim 5, it is characterised in that：Material containing magnesium
Addition be converted to MgCl by the magnesium in material containing magnesium21-3 times of theoretical amount determine, NH4A concentration of 1.5- of Cl solution
15mol/L, the temperature for mixing reaction thoroughly are 0-150 DEG C, reaction time 0.5-5.5h.
7. a kind of method of normal pressure short route production magnesium hydroxide according to claim 6, it is characterised in that：It is stirred to react
When rising to 4.5-9.4 to pH value of solution, oxidizing agent scavenging removal of impurities is added, filters to contain MgCl2Refined brine.
8. a kind of method of normal pressure short route production magnesium hydroxide according to claim 7, it is characterised in that：The oxidation
Agent is selected from least one of hydrogen peroxide, calcium hypochlorite, magnesium hypochlorite, chlorine.
9. a kind of method of normal pressure short route production magnesium hydroxide according to claim 4-8 any one, feature exist
In：The gas collection reuse refers to that the gas for generating reaction is introduced directly into containing MgCl2Brine or refined brine or magnesium sinking
Afterwards in liquid, or through lime removing CO therein2It is imported again containing MgCl afterwards2Brine or refined brine or magnesium sinking after in liquid, be allowed to turn
It is melted into NH4Cl, or be allowed to be converted to NH with hydrochloric acid or calcium chloride solution absorption4Cl is recycled in process.
10. a kind of method of normal pressure short route production magnesium hydroxide according to any one of claims 1 to 8, feature exist
In：It is passed through CO into liquid after the magnesium sinking2Gas is used in combination ammonia to adjust pH value of solution to 3.5-8.5, and 0~60 DEG C of reaction 0.5~
6.5h filters to obtain calcium carbonate filter cake and regeneration ammonium chloride solution, and gained, which regenerates ammonium chloride solution and returns, contains MgCl2Making from brine it is standby
Process recycles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810203171.2A CN108439441A (en) | 2018-03-13 | 2018-03-13 | A kind of method of normal pressure short route production magnesium hydroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810203171.2A CN108439441A (en) | 2018-03-13 | 2018-03-13 | A kind of method of normal pressure short route production magnesium hydroxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108439441A true CN108439441A (en) | 2018-08-24 |
Family
ID=63194830
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810203171.2A Pending CN108439441A (en) | 2018-03-13 | 2018-03-13 | A kind of method of normal pressure short route production magnesium hydroxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108439441A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574174A (en) * | 2018-12-13 | 2019-04-05 | 中南大学 | A kind of method that rare-earth smelting technical process chlorine-contained wastewater is administered |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362603A (en) * | 2008-09-03 | 2009-02-11 | 河北科技大学 | High purity magnesium hydrate preparation method |
| CN102417196A (en) * | 2011-09-16 | 2012-04-18 | 沈阳化工大学 | Production method of fire retardant type magnesium hydroxide |
| KR20130039836A (en) * | 2011-10-13 | 2013-04-23 | 충북대학교 산학협력단 | Synthesis of nano sized magnesium hydroxide |
| CN107032384A (en) * | 2017-06-05 | 2017-08-11 | 中南大学 | A kind of method that calcium and magnesium is separated and recovered from Calcium magnesium minerals |
-
2018
- 2018-03-13 CN CN201810203171.2A patent/CN108439441A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362603A (en) * | 2008-09-03 | 2009-02-11 | 河北科技大学 | High purity magnesium hydrate preparation method |
| CN102417196A (en) * | 2011-09-16 | 2012-04-18 | 沈阳化工大学 | Production method of fire retardant type magnesium hydroxide |
| KR20130039836A (en) * | 2011-10-13 | 2013-04-23 | 충북대학교 산학협력단 | Synthesis of nano sized magnesium hydroxide |
| CN107032384A (en) * | 2017-06-05 | 2017-08-11 | 中南大学 | A kind of method that calcium and magnesium is separated and recovered from Calcium magnesium minerals |
Non-Patent Citations (4)
| Title |
|---|
| 全跃 等: "《镁质材料生产与应用》", 29 February 2008, 冶金工业出版社 * |
| 徐采栋: "《碱性热风化铁炉与碱性转炉炼钢》", 31 January 1960, 贵州人民出版社 * |
| 王迎军 等: "《新型材料科学与技术 无机材料卷（中册）》", 31 October 2016, 华南理工大学出版社 * |
| 韩行禄: "《不定形耐火材料》", 31 January 2003, 冶金工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574174A (en) * | 2018-12-13 | 2019-04-05 | 中南大学 | A kind of method that rare-earth smelting technical process chlorine-contained wastewater is administered |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101759765B1 (en) | Production of high purity precipitated calcium carbonate | |
| CN103011203B (en) | Method for treatment of chlorinated waste molten salt generated in TiCl4 production process | |
| CN101348268B (en) | Two comprehensive methods of utilization of boron mud, giobertite and talc deposit for preparing magnesia and silicon dioxide | |
| CA2756763C (en) | Process for simultaneous production of potassium sulphate, ammonium sulfate, magnesium hydroxide and/or magnesium oxide from kainite mixed salt and ammonia | |
| CN102225775A (en) | Process for producing magnesium hydroxide and calcium carbonate by dolomite conversion method | |
| CN101607720A (en) | With the bittern that contains magnesium chloride is the feedstock production method of magnesium oxide | |
| CN109047285A (en) | Containing sodium, the method for transformation of fluorochemical and system in a kind of waste cathode of aluminum electrolytic cell carbon block | |
| CN101172627B (en) | Method of producing magnesium hydroxide | |
| CA2794975A1 (en) | Production of calcium carbonate from waste sludge | |
| CN112551561A (en) | Method for producing active magnesium oxide from waste residues of spices | |
| CN102515221A (en) | Method for extracting alumina and amorphous silica from fly ash or coal gangue | |
| CN104591234A (en) | Process for preparing light magnesium carbonate from industrial magnesium hydroxide | |
| CN114180604A (en) | Comprehensive utilization method of waste residues in spice production and synthetic ammonia purge gas | |
| CN101374767B (en) | An improved process for preparation of magnesium oxide | |
| CN107032384A (en) | A kind of method that calcium and magnesium is separated and recovered from Calcium magnesium minerals | |
| CN109694092A (en) | A kind of comprehensive processing method of the solid waste containing chlorine | |
| CN106745582A (en) | A kind of method that sial slag prepares polyaluminum silicate chloride coagulant | |
| KR20170004915A (en) | The manufacturing method of magnesium carbonate and calcium chloride using dolomite for raw material | |
| CN101157464B (en) | Dolomite wet process comprehensive utilization technique | |
| CN108439441A (en) | A kind of method of normal pressure short route production magnesium hydroxide | |
| CN1098382A (en) | The method of preparation of hydrocarbon calcium carbonate by acid decomposition reclaiming circulation | |
| CN102285677A (en) | Method for producing calcium chloride based on carbide slag as raw material | |
| CN102838141A (en) | Process for producing magnesium hydrate by removing silicon and aluminum from magnesite | |
| CN105883864A (en) | Method for producing basic magnesium carbonate from boron mud waste material | |
| CN101723431A (en) | Method for recovering magnesium from magnesium sulfate solution |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180824 |