CN106644669B - A kind of cigarette combustion cone fixing means and device - Google Patents

A kind of cigarette combustion cone fixing means and device Download PDF

Info

Publication number
CN106644669B
CN106644669B CN201611127086.XA CN201611127086A CN106644669B CN 106644669 B CN106644669 B CN 106644669B CN 201611127086 A CN201611127086 A CN 201611127086A CN 106644669 B CN106644669 B CN 106644669B
Authority
CN
China
Prior art keywords
cigarette
combustion cone
dodecenylsuccinic anhydride
embedding
dehydration
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
CN201611127086.XA
Other languages
Chinese (zh)
Other versions
CN106644669A (en
Inventor
王亮
银董红
谢国勇
杜文
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.)
China Tobacco Hunan Industrial Co Ltd
Original Assignee
China Tobacco Hunan Industrial 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 China Tobacco Hunan Industrial Co Ltd filed Critical China Tobacco Hunan Industrial Co Ltd
Priority to CN201611127086.XA priority Critical patent/CN106644669B/en
Publication of CN106644669A publication Critical patent/CN106644669A/en
Application granted granted Critical
Publication of CN106644669B publication Critical patent/CN106644669B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/36Embedding or analogous mounting of samples
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/42Low-temperature sample treatment, e.g. cryofixation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2873Cutting or cleaving

Abstract

The invention discloses a kind of cigarette combustion cone fixing means and devices.The present invention obtains cigarette combustion cone internal structure by situ, the defect of in-situ observation can not be carried out to cigarette combustion cone partial interior microstructure by overcoming conventional method, the microstructure for remaining cigarette combustion cone to the maximum extent, the mechanism generated for further investigation cigarette burning process and harmful substance provide foundation.

Description

A kind of cigarette combustion cone fixing means and device
Technical field
The present invention relates to a kind of cigarette combustion cone fixing means and devices, belong to cigarette field.
Background technique
The aroma source of cigarette is burnt and also produces a large amount of harmful components simultaneously in combustion process, these it is harmful at The generation and combustion state divided is closely related, therefore has for the research of combustion state for tobacco business reducing tar and reducing harm important Directiveness effect.
For a long time, slow for the microstructure change progress during cigarette burning, essentially consist in cigarette knot The particularity of structure, burning wimble fraction pipe tobacco brittleness is very big, and burning poppet surface and internal structure are highly vulnerable to breakage during cutting, therefore And it is difficult to carry out the internal structure of combustion cone anatomy observation in situ.Therefore it finds a kind of simple and effective and can see in situ Examine internal microstructure changes during cigarette burning Method means very it is necessary to.
Summary of the invention
It is simple, efficient, accurate that the object of the present invention is to provide one kind, retains the form knot of cigarette combustion cone to greatest extent Structure, the cigarette combustion cone fixing means in situ for obtaining cigarette combustion cone internal structure.
Simply retain the morphosis of cigarette combustion cone to greatest extent another object of the present invention is to provide a kind of, and Efficiently, accurately the cigarette combustion cone in situ for obtaining cigarette combustion cone internal structure fixes device.
A method of it is in situ to obtain cigarette combustion cone internal structure, the cigarette of combustion state is not being influenced into combustion cone knot Extinguish rapidly under the premise of structure, go to grey part of exchanging, is subsequently placed in -10 DEG C~-5 DEG C freezen protectives;Burning tapered end is placed in packet In pipe laying, embedding medium I is slowly added dropwise under the premise of not influencing to burn wimble structure, stands infiltration, embedding is then further added dropwise Agent II is heated to 40-80 DEG C, solidifies 6-48h, cutting, observation;
The ingredient of the embedding medium I are as follows: 1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol Acrylamide;
Each component molar ratio are as follows: 1,2,3- means of dehydration of glycerol glycerin ether/(dodecenylsuccinic anhydride+N- methylol propylene Amide)=1/0.69, wherein dodecenylsuccinic anhydride/N hydroxymethyl acrylamide ratio range is 0.1-0.5;
The ingredient of the embedding medium II are as follows: 1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol Acrylamide and 2,4,6- tri- (dimethylamino methyl) phenol;
Each component molar ratio are as follows: 1,2,3- means of dehydration of glycerol glycerin ether/(dodecenylsuccinic anhydride+N- methylol propylene Amide)/2,4,6- tri- (dimethylamino methyl) phenol=1:0.69:0.01, wherein dodecenylsuccinic anhydride/N- methylol third Acrylamide=0.1-0.5.
The molar ratio of the dodecenylsuccinic anhydride and N hydroxymethyl acrylamide is preferably 0.25-0.45.
Preferably, burning tapered end is placed in embedding pipe in the case where cigarette vertically being fixed.
The cigarette of combustion state is preferably placed in small-sized closed container by the method extinguished rapidly.
It can not only quickly extinguish in this way, and be conducive to maintain original burning wimble structure.
The small-sized closed container is preferably glass bushing.
By using glass bushing, help quickly to extinguish.
The time of penetration is preferably 1-4 hours.
By the way that within the above range, optimal osmotic effect can be reached, reduces the generation of bubble time of penetration control, And the burning wimble structure of cigarette is not destroyed simultaneously.
The solidification temperature is preferably 60-80 DEG C.
The curing time is preferably 6-12 hours.
By control solidification temperature and curing time, the embedding effect that can have further obtained.
Preferably rectangular in shape, square, the round or triangle of used embedding pipe.
The mode of the observation includes directly observing combustion cone cross-section structure, passing through optical microscopy, scanning electron microscopy Mirror, transmission electron microscope or confocal laser scanning microscope.
Device, including pedestal are fixed used in above-mentioned cigarette combustion cone fixing means, the pedestal is equipped with embedding pipe Bracket;Embedding pipe is installed on the embedding pipe holder;The embedding tube opening is vertically arranged upward;It is also installed on the pedestal There is the cigarette clamper that can steadily move up and down;Make after the cigarette clamper clamping cigarette cigarette be located at embedding pipe just on Side, and combustion cone is rectified to embedding tube opening end.
The embedding pipe holder can stretch up and down, to adjust cigarette embedding length, meanwhile, in same sample displacement embedding medium In the process, also facilitate adjusting embedding pipe height or replacement embedding pipe.
The embedding pipe preferably has the structure for adapting to cigarette shape.
Facilitate to agree with cigarette and glass bushing preferably in this way.
The outer shape of the embedding pipe is preferably rectangle, square, circle or triangle.
The internal diameter of the embedding pipe is preferably 8mm~12mm.
It is defined by the internal diameter to embedding pipe, can further match cigarette dimension, while reducing the use of embedding medium Amount.
Advantages of the present invention essentially consists in:
The problem of can not carrying out in-situ observation to cigarette combustion cone partial internal structure the invention avoids conventional method, most The microstructure for remaining to limits cigarette combustion cone, the machine generated for further investigation cigarette burning process and harmful substance System provides foundation.
By means of the present invention, the microstructure for each position of combustion cone during home position observation cigarette burning provides Feasibility, avoids the disadvantages of direct cutting process of combustion cone is frangible, during remaining cigarette burning to the maximum extent Actual physical state.Meanwhile obtained sample can be further sliced, polishing treatment, directly be observed, or transmission electricity The means such as mirror, scanning electron microscope, laser confocal microscope are observed and are analyzed with carrying out high-resolution, to fire from microcosmic angle to cigarette Burning process carries out analysis and provides necessary means.
In specific scheme, by carrying out strict control to whole process and parameter, including the selection to embedding medium, ingeniously Two steps of application embed wonderfully, and composition proportion and entire sampling, embedding, solidification process are continued to optimize, and just obtain this hair It is bright that efficiently, accurately original position obtains the effect of cigarette combustion cone internal structure.
The solidification effect especially of the invention just obtained in a short period of time, can largely shorten preparation Period improves efficiency.
As shown in attached drawing of the invention, observed by the slice that microscope obtains the present invention, various sections Structure is all very clear.And it can accurately measure the Areal porosity of gained combustion cone.
The device of the invention is simple, and structure is simple and convenient to operate, and is each position during home position observation cigarette burning Microstructure provides feasibility, avoids the disadvantages of combustion cone cutting process is frangible, remains cigarette burning to the maximum extent Actual physical state in the process;Meanwhile cigarette and embedding pipe are relatively fixed, avoid since cigarette density is small, can not be complete Immerse phenomena such as embedding caused by embedding medium is incomplete;Obtained sample can further be sliced, polishing treatment, be transmitted The means such as Electronic Speculum, scanning electron microscope, laser confocal microscope are observed and are analyzed with carrying out high-resolution, can be from microcosmic angle pair Cigarette burning process carries out analysis and provides necessary means.
Detailed description of the invention
Fig. 1 is the cigarette combustion cone slice along the axially cutting acquisition of cigarette.
Fig. 2 is the cigarette combustion cone slice that transverse cuts obtain.
Fig. 3 is cigarette combustion cone center axial slice.
Can be seen that the present invention from Fig. 1-Fig. 3 can obtain the structure of gem-pure each section.Including charred portion The structure of non-charred portion is very clear.
Fig. 4 is the schematic diagram of the fixed device of cigarette combustion cone used in the present invention.
Specific embodiment
Following embodiment is intended to illustrate invention, rather than further limits to the scope of the present invention.
Embodiment 1
It is as follows that cigarette combustion cone embeds fixing step:
(1) it samples: taking a cigarette sample to light, third mouth is pumped under mode standard, cigarette is put into circle rapidly In glass bushing, extinguish cigarette rapidly.Grey part of exchanging carefully is gone to, cigarette is placed in freezen protective at -10 DEG C~-5 DEG C and is waited for With.
(2) it embeds: by embedding medium I:1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol third Acrylamide is uniformly mixed according to molar ratio for 1:0.2:0.49, and cigarette is vertically fixed, and burning tapered end is placed in embedding pipe.Slowly Embedding medium I is instilled, permeate 2 hours under room temperature, is then slowly dropped into embedding medium II, is respectively formulated and ratio is as follows: 1,2,3- the third three Dehydration of alcohols glycerin ether, dodecenylsuccinic anhydride, N hydroxymethyl acrylamide and 2,4,6- tri- (dimethylamino methyl) phenol Molar ratio be 1:0.2:0.49:1.
(3) solidify: being placed in baking oven, solidify 12 hours at 60 DEG C.
(4) it cuts: the cigarette sample after solidification being taken out from embedding pipe, removes and does not embed part.Use precision slicer Cutting is carried out, the axial cross section of cigarette combustion cone is obtained.
The microscope observation analysis of cigarette combustion cone
The cigarette combustion cone embedded samples of acquisition are subjected to axially cutting, slice thickness 0.1mm (Fig. 3).It is aobvious to be placed in optics Micro- microscopic observation combustion cone internal structure distinguishes its combustion state and distribution by pipe tobacco color.Combustion cone length is measured simultaneously 11.58mm, area of section 56.22mm2, and the volume for calculating combustion cone is about 512.36mm3.Pass through the images such as Image J Processing software, the Areal porosity for calculating the cigarette sample combustion cone is 33.2%, significantly less than the Areal porosity of unburned part 50.1%.
Embodiment 2
As shown in figure 4, the fixed device of cigarette combustion cone of the invention, including pedestal 1, the pedestal 1 are equipped with embedding pipe Bracket 6;Outer shape is installed for round, square or triangle on the embedding pipe holder 6, internal diameter is 8mm~12mm's Embed pipe 5;The embedding pipe 5 is opening up to be vertically arranged;The cigarette folder that can steadily move up and down is also equipped on the pedestal 1 Holder 2;The cigarette clamper clamps the surface for making cigarette 3 be located at embedding pipe after cigarette 3, and combustion cone is rectified to embedding pipe 5 open ends.
In use, a cigarette sample is taken to light first, it is pumped to third mouth under mode standard, cigarette is put into circle rapidly In shape glass bushing, extinguish cigarette rapidly;Grey part of exchanging carefully is gone to, cigarette 3 is fixed on vertically in cigarette clamper 2, And height is regulated, protrude into combustion cone 4 integrally in embedding pipe 5;It is slowly dropped into the embedding medium for being not added with curing agent, is seeped under room temperature Saturating 2 hours;Then the height of embedding pipe holder 6 is adjusted, the embedding pipe more renewed makes combustion cone 4 integrally protrude into the packet after replacement In pipe laying, and fill the embedding medium containing curing agent of brand-new;After standing eliminates bubble, whole device is placed in baking oven, 60 Solidify 24 hours at DEG C;The cigarette sample after solidification is taken out from embedding pipe finally, removes and does not embed part;Use precision slicing Machine carries out cutting, obtains the axial cross section of cigarette combustion cone, and carry out subsequent analysis.
Comparative example 1
It in step (2), is directly handled with embedding medium II, is not used embedding medium I, remaining step is with embodiment 1, as a result Generate a large amount of bubbles, can not accurate observation combustion cone structure.

Claims (6)

1. a kind of cigarette combustion cone fixing means, which is characterized in that extinguish the cigarette of combustion state rapidly, go to grey portion of exchanging Point, it is subsequently placed in -10 DEG C~-5 DEG C freezen protectives;Embedding medium I is added dropwise, stands infiltration, embedding medium II is then further added dropwise, adds Heat solidifies 6-48h, cutting, observation to 40-80 DEG C;
The ingredient of the embedding medium I are as follows: 1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol propylene Amide;
Each component molar ratio are as follows: 1,2,3- means of dehydration of glycerol glycerin ether/(dodecenylsuccinic anhydride+N hydroxymethyl acrylamide) =1/0.69, wherein dodecenylsuccinic anhydride/N hydroxymethyl acrylamide=0.1-0.5;
The ingredient of the embedding medium II are as follows: 1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol propylene Amide and 2,4,6- tri- (dimethylamino methyl) phenol;
Each component molar ratio are as follows: 1,2,3- means of dehydration of glycerol glycerin ether/(dodecenylsuccinic anhydride+N- methylol acryloyl Amine)/2,4,6- tri- (dimethylamino methyl) phenol=1:0.69:0.01, wherein dodecenylsuccinic anhydride/N- methylol propylene Amide=0.1-0.5.
2. according to the method described in claim 1, it is characterized by: the dodecenylsuccinic anhydride and N- methylol acryloyl The molar ratio of amine is 0.25-0.45.
3. method according to claim 1 or 2, it is characterised in that: the time of the infiltration is 1-4 hours.
4. method according to claim 1 or 2, it is characterised in that: the cured temperature is 60-80 DEG C, when cured Between be 6-12 hours.
5. the method according to claim 1, it is characterised in that: burning tapered end is placed in embedding in the case where cigarette is vertically fixed Guan Zhong.
6. the method according to claim 1, it is characterised in that: the method extinguished rapidly is small-sized for the cigarette of combustion state to be placed in In closed container, the small-sized closed container is glass bushing.
CN201611127086.XA 2016-12-09 2016-12-09 A kind of cigarette combustion cone fixing means and device Active CN106644669B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611127086.XA CN106644669B (en) 2016-12-09 2016-12-09 A kind of cigarette combustion cone fixing means and device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611127086.XA CN106644669B (en) 2016-12-09 2016-12-09 A kind of cigarette combustion cone fixing means and device

Publications (2)

Publication Number Publication Date
CN106644669A CN106644669A (en) 2017-05-10
CN106644669B true CN106644669B (en) 2019-06-11

Family

ID=58824071

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201611127086.XA Active CN106644669B (en) 2016-12-09 2016-12-09 A kind of cigarette combustion cone fixing means and device

Country Status (1)

Country Link
CN (1) CN106644669B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108303344B (en) * 2017-12-20 2020-04-17 红云红河烟草(集团)有限责任公司 Method for judging falling of cigarette combustion cone

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4854332A (en) * 1986-07-03 1989-08-08 Sakura Color Products Corp. Cigarette having thermochromogenic portions thereon
CN101815934A (en) * 2007-09-16 2010-08-25 莱卡生物系统努斯洛赫有限责任公司 Tissue infiltration device
CN203355767U (en) * 2013-07-05 2013-12-25 陕西科技大学 Embedding pipe bracket
CN104824840A (en) * 2015-03-12 2015-08-12 红云红河烟草(集团)有限责任公司 Cigarette core capable of preventing cigarette burning cone from dropping and method for manufacturing same
CN105158142A (en) * 2015-09-16 2015-12-16 中国烟草总公司郑州烟草研究院 Detection method for permeability of cigarette burning cone
CN105651626A (en) * 2015-12-23 2016-06-08 中国烟草总公司郑州烟草研究院 Automatic control detection device and detection method for cigarette combustion coal fall-off performance
CN205426882U (en) * 2015-10-27 2016-08-03 云南中烟工业有限责任公司 Bullet cigarette ash device of rate tester that drops is bored in burning to tobacco equipment

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4854332A (en) * 1986-07-03 1989-08-08 Sakura Color Products Corp. Cigarette having thermochromogenic portions thereon
CN101815934A (en) * 2007-09-16 2010-08-25 莱卡生物系统努斯洛赫有限责任公司 Tissue infiltration device
CN203355767U (en) * 2013-07-05 2013-12-25 陕西科技大学 Embedding pipe bracket
CN104824840A (en) * 2015-03-12 2015-08-12 红云红河烟草(集团)有限责任公司 Cigarette core capable of preventing cigarette burning cone from dropping and method for manufacturing same
CN105158142A (en) * 2015-09-16 2015-12-16 中国烟草总公司郑州烟草研究院 Detection method for permeability of cigarette burning cone
CN205426882U (en) * 2015-10-27 2016-08-03 云南中烟工业有限责任公司 Bullet cigarette ash device of rate tester that drops is bored in burning to tobacco equipment
CN105651626A (en) * 2015-12-23 2016-06-08 中国烟草总公司郑州烟草研究院 Automatic control detection device and detection method for cigarette combustion coal fall-off performance

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Numerical simulation of a burning cigarette during puffing;Mohammad S. Saidi et al.;《J. Anal. Appl. Pyrolysis》;20040609;第72卷;第141-152页
卷烟燃烧锥受力分析与落头倾向检测方法;李斌 等;《烟草工艺》;20141231(第1期);第12-15页

Also Published As

Publication number Publication date
CN106644669A (en) 2017-05-10

Similar Documents

Publication Publication Date Title
CN106644669B (en) A kind of cigarette combustion cone fixing means and device
EP2570075A3 (en) Numerical aperture (na) controlling unit, variable optical probe including the na controlling unit, and depth scanning method using the na controlling unit
WO2008051937A3 (en) Method for creating s/tem sample and sample structure
US20150138532A1 (en) Motion strategies for scanning microscope imaging
Mohsin et al. Microcracks in compact bone: a three‐dimensional view
EP2299307A3 (en) Cytological imaging method
CN102879330A (en) In-situ tracking metallographic analysis method for microstructural evolution of steels
TW201713930A (en) Method for preparing a sample for microstructure diagnostics, and sample for microstructure diagnostics
TWI277730B (en) Laser beam incident optical device
CN106768440B (en) Method and device that is a kind of while obtaining cigarette burning wimble structure and Temperature Distribution
US20210025789A1 (en) Tissue sectioning system
Mac 3D characterisation of microcracks in concrete
Wang et al. Transverse and axial resolution of femtosecond laser ablation
EP2110699A3 (en) Method and device for lighting an object scene
Nguyen et al. Control of femtosecond laser written waveguides in silica glass
EP2914951B1 (en) 3d laser ablation tomography and spectrographic analysis
JP2013224927A (en) Observation sample, observation sample preparation method, and observation method
US20080318265A1 (en) Measuring the Thickness of Organic Samples
CN206235500U (en) A kind of simple cigarette embedding fixing device
Jimson et al. Artifact in histological section
Westfall et al. A water control device for mounting serial ultrathin sections
Boutilier et al. Development of an auto-interchangeable multi-pinhole array for confocal laser scanning microscopy systems using precision laser processing
CN107102017B (en) The method that same sample is observed using paraffin section and scanning electron microscope
Orchard et al. Use of softening agents to improve the production of formalin-fixed, paraffin-embedded sections of nail tissue: an assessment
Gologan et al. Factors influencing the quality of formaldehyde fixed paraffin embedded tissue samples—Review

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