CN108929568A - A kind of preparation method of the silicon carbide powder as organic composite material reinforcement - Google Patents
A kind of preparation method of the silicon carbide powder as organic composite material reinforcement Download PDFInfo
- Publication number
- CN108929568A CN108929568A CN201810945540.5A CN201810945540A CN108929568A CN 108929568 A CN108929568 A CN 108929568A CN 201810945540 A CN201810945540 A CN 201810945540A CN 108929568 A CN108929568 A CN 108929568A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- carbide powder
- composite material
- organic composite
- preparation
- 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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention belongs to technical field of preparation for inorganic material, and disclose a kind of preparation method of silicon carbide powder as organic composite material reinforcement, comprising the following steps: silicon carbide powder raw material are sent into ball mill carry out Shape correction first；Then, orthopedic silicon carbide powder is preheated into 20min~30min at 60 DEG C~80 DEG C, modifying agent is sprayed onto the silicon carbide powder of high-speed stirred with mist every time, controlled at 100 DEG C~120 DEG C, dry 2h~the 3h of every stirring stands 20min~30min, stirring 4 times, the silicon carbide powder being tentatively modified；Finally, tentatively modified silicon carbide powder dip-coating in hardening agent is obtained modified silicon carbide powder.The present invention can be effectively improved the compatibility of silicon carbide powder and organic composite material, improve compatibility and dispersibility when its filling, improve the comprehensive performance of product, and simple process, be easy to control.
Description
Technical field
The invention belongs to technical field of preparation for inorganic material, in particular to a kind of carbon as organic composite material reinforcement
SiClx raw powder's production technology.
Background technique
Organic composite material is widely used at present, but since its own wearability is not outstanding, thermal conductivity is not good enough yet, part
Organic composite industrial products have the two indexs harsh requirement, for the index performance for further enhancing material, are added
Suitable reinforcing material is imperative.
Silicon carbide has inoxidizability strong, and wear-resisting property is good, and hardness is high, and thermal stability is good, and elevated temperature strength is big, thermal expansion system
Number is small, and thermal conductivity is big and anti-thermal shock and equal good characteristics resistant to chemical etching, is widely used in function ceramics, advanced fire proofed wood
Expect, serve as the numerous areas such as reinforcement.Silicon carbide be used as reinforcement organic composite material when, due to silicon carbide belong to it is inorganic non-
Metal material, molecular structure are ionic bond crystal, have good hydrophily, and organic composite material surface is modified property mostly
, this results in silicon carbide that cannot fill in organic composite material well, needs through special modification, Cai Nenggeng
Good combines with organic composite material, achievees the purpose that enhance organic composite material.When silicon carbide is as organic composite material
Reinforcement when, how to improve the compatibility between silicon carbide and organic composite material, be current urgent problem.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of silicon carbide powder as organic composite material reinforcement.
To achieve the goals above, the technical solution that the application uses are as follows: a kind of as organic composite material reinforcement
The preparation method of silicon carbide powder, comprising the following steps:
(1) silicon carbide powder raw material is sent into ball mill and carries out Shape correction 30min~40min, taken out, it is spare；
(2) the orthopedic silicon carbide powder of step (1) is preheated at 60 DEG C~80 DEG C 20min~30min, will changed every time
Property agent is sprayed onto the silicon carbide powder of high-speed stirred with mist, and controlled at 100 DEG C~120 DEG C, mixing speed is
300r/min~600r/min, the dry 2h~3h of every stirring stand 20min~30min, are placed in baking oven for stirring 4 times and to dry,
The silicon carbide powder being tentatively modified；
The modifying agent be aminopropyl triethoxysilane, methacryloxypropyl trimethoxy silane, ethyl alcohol and
The mixed solution of water, wherein the weight percent of each ingredient is respectively aminopropyl triethoxysilane 10%~15%, methyl-prop
Alkene acryloxypropylethoxysilane trimethoxy silane 5%~10%, ethyl alcohol 65%~70% and excess water；
(3) tentatively modified silicon carbide powder after dip-coating 10s~50s, is dried in an oven in hardening agent；It is wherein strong
Agent is the mixture of silane coupling agent and polyethyleneimine amide, and the weight ratio of silane coupling agent and polyethyleneimine amide is 2:3
~5.
Further, ball mill draw ratio described in step (1) is less than 3.
Further, SiC content is not less than 98% in the silicon carbide powder raw material.
Further, the median grain diameter of the orthopedic silicon carbide powder of step (1) is D50It is 1.5 μm~2.5 μm.
Further, in the modifying agent weight percent of each ingredient be respectively aminopropyl triethoxysilane 10%,
Methacryloxypropyl trimethoxy silane 10%, ethyl alcohol 70% and excess water.
Further, the weight ratio of the silane coupling agent and polyethyleneimine amide is 2:3.
Compared with prior art, the beneficial effects of the present invention are:
(1) after carrying out surface shaping in the ball mill, the shape rounding of silicon carbide powder, without sharp corners, as multiple
Condensation material reinforcing agent can be obviously improved composite property, avoid sharp granule-morphology to the mobility and material system of powder
The plasticity of product has an impact.
(2) hydrophobic modified, the hydrophilic group and silicon carbide of modifying agent are first carried out to silicon carbide powder surface using modifying agent
Physical and chemical effect occurs for powder surface, forms absorption, and outwardly, powder surface becomes hydrophobicity from hydrophily to lipophilic group, so as to improve
The compatibility of silicon carbide powder and organic composite material improves compatibility and dispersibility when its filling, improves the synthesis of product
Performance is modified twice, reaches effect more.Afterwards using hardening agent in order to ensure modified silicon carbide powder is hydrophobic
Stability.
Specific embodiment
Technological means of the invention, creation characteristic, achieving the goal is easy to understand with effect in order to make, below in conjunction with
Technical solution of the present invention is clearly and completely described in the embodiment of the present invention.
Below in conjunction with specific embodiment, the present invention is described further:
Embodiment 1
A kind of preparation method of the silicon carbide powder as organic composite material reinforcement, comprising the following steps:
(1) it takes the silicon carbide powder raw material that SiC content is 98% to be sent into the ball mill that draw ratio is 2.5 to carry out at shaping
30min is managed, is taken out, it is spare；The median grain diameter of silicon carbide powder after obtained shaping is D50It is 1.5 μm~2 μm.
(2) orthopedic silicon carbide powder is preheated at 60 DEG C 20min, modifying agent is sprayed onto height with mist every time
In the silicon carbide powder of speed stirring, controlled at 100 DEG C, mixing speed 300r/min, the dry 2h of every stirring is stood
20min is stirred 4 times and is placed in baking oven the silicon carbide powder dried, be tentatively modified；
Modifying agent is aminopropyl triethoxysilane, methacryloxypropyl trimethoxy silane, second alcohol and water
Mixed solution, wherein the weight percent of each ingredient is respectively aminopropyl triethoxysilane 10%, methacryloxy third
Base trimethoxy silane 5%, ethyl alcohol 65% and water 20%；
(3) tentatively modified silicon carbide powder after dip-coating 10s, is dried in an oven in hardening agent；Wherein hardening agent
For the mixture of silane coupling agent and polyethyleneimine amide, the weight ratio of silane coupling agent and polyethyleneimine amide is 2:4.
Treatment effect: untreated preceding silicon carbide powder moistening height is 2.52, and maximum volume solid concentration is 38.72%；
Obtained silicon carbide powder moistening height is 6.7 after processing, and maximum volume solid concentration is 51.67%.
Embodiment 2
A kind of preparation method of the silicon carbide powder as organic composite material reinforcement, comprising the following steps:
(1) it takes the silicon carbide powder raw material that SiC content is 98.5% to be sent into the ball mill that draw ratio is 2 to carry out at shaping
40min is managed, is taken out, it is spare；The median grain diameter of silicon carbide powder after obtained shaping is D50It is 1 μm~1.5 μm.
(2) orthopedic silicon carbide powder is preheated at 80 DEG C 30min, modifying agent is sprayed onto height with mist every time
In the silicon carbide powder of speed stirring, controlled at 120 DEG C, mixing speed 600r/min, the dry 3h of every stirring is stood
30min is stirred 4 times and is placed in baking oven the silicon carbide powder dried, be tentatively modified；
Modifying agent is aminopropyl triethoxysilane, methacryloxypropyl trimethoxy silane, second alcohol and water
Mixed solution, wherein the weight percent of each ingredient is respectively aminopropyl triethoxysilane 15%, methacryloxy third
Base trimethoxy silane 10%, ethyl alcohol 68% and water 7%；
(3) tentatively modified silicon carbide powder after dip-coating 50s, is dried in an oven in hardening agent；Wherein hardening agent
For the mixture of silane coupling agent and polyethyleneimine amide, the weight ratio of silane coupling agent and polyethyleneimine amide is 2:5.
Treatment effect: untreated preceding silicon carbide powder moistening height is 3.17, and maximum volume solid concentration is 38.92%；
Obtained silicon carbide powder moistening height is 7.0 after processing, and maximum volume solid concentration is 53.17%.
Embodiment 3
A kind of preparation method of the silicon carbide powder as organic composite material reinforcement, comprising the following steps:
(1) it takes the silicon carbide powder raw material that SiC content is 99% to be sent into the ball mill that draw ratio is 2.8 to carry out at shaping
35min is managed, is taken out, it is spare；The median grain diameter of silicon carbide powder after obtained shaping is D50It is 1.5 μm~2.5 μm.
(2) orthopedic silicon carbide powder is preheated at 70 DEG C 25min, modifying agent is sprayed onto height with mist every time
In the silicon carbide powder of speed stirring, controlled at 110 DEG C, mixing speed 450r/min, the dry 2.5h of every stirring is stood
25min is stirred 4 times and is placed in baking oven the silicon carbide powder dried, be tentatively modified；
Modifying agent is aminopropyl triethoxysilane, methacryloxypropyl trimethoxy silane, second alcohol and water
Mixed solution, wherein the weight percent of each ingredient is respectively aminopropyl triethoxysilane 10%, methacryloxy third
Base trimethoxy silane 10%, ethyl alcohol 70% and water 10%；
(3) tentatively modified silicon carbide powder after dip-coating 30s, is dried in an oven in hardening agent；Wherein hardening agent
For the mixture of silane coupling agent and polyethyleneimine amide, the weight ratio of silane coupling agent and polyethyleneimine amide is 2:3.
Treatment effect: untreated preceding silicon carbide powder moistening height is 2.91, and maximum volume solid concentration is 35.47%；
Obtained silicon carbide powder moistening height is 6.8 after processing, and maximum volume solid concentration is 52.09%.
Disclosed above is only presently preferred embodiments of the present invention, and still, the embodiment of the present invention is not limited to this, Ren Heben
What the technical staff in field can think variation should all fall into protection scope of the present invention.
Claims (6)
1. a kind of preparation method of the silicon carbide powder as organic composite material reinforcement, which is characterized in that including following step
It is rapid:
(1) silicon carbide powder raw material is sent into ball mill and carries out Shape correction 30min~40min, taken out, it is spare；
(2) orthopedic silicon carbide powder is preheated to 20min~30min at 60 DEG C~80 DEG C, every time by modifying agent with mist
Form is sprayed onto the silicon carbide powder of high-speed stirred, controlled at 100 DEG C~120 DEG C, mixing speed be 300r/min~
600r/min, the dry 2h~3h of every stirring stand 20min~30min, are placed in baking oven for stirring 4 times and to dry, are tentatively changed
The silicon carbide powder of property；
The modifying agent is aminopropyl triethoxysilane, methacryloxypropyl trimethoxy silane, second alcohol and water
Mixed solution, wherein the weight percent of each ingredient is respectively aminopropyl triethoxysilane 10%~15%, methacryl
Oxygroup propyl trimethoxy silicane 5%~10%, ethyl alcohol 65%~70% and excess water；
(3) tentatively modified silicon carbide powder after dip-coating 10s~50s, is dried in an oven in hardening agent；Wherein hardening agent
For the mixture of silane coupling agent and polyethyleneimine amide, the weight ratio of silane coupling agent and polyethyleneimine amide is 2:3~5.
2. the preparation method of the silicon carbide powder as described in claim 1 as organic composite material reinforcement, feature exist
In ball mill draw ratio described in step (1) is less than 3.
3. the preparation method of the silicon carbide powder as described in claim 1 as organic composite material reinforcement, feature exist
In SiC content is not less than 98% in the silicon carbide powder raw material.
4. the preparation method of the silicon carbide powder as described in claim 1 as organic composite material reinforcement, feature exist
In the median grain diameter of the orthopedic silicon carbide powder of step (1) is D50It is 1.5 μm~2.5 μm.
5. the preparation method of the silicon carbide powder as described in claim 1 as organic composite material reinforcement, feature exist
In the weight percent of each ingredient is respectively aminopropyl triethoxysilane 10%, methacryloxy in the modifying agent
The water of propyl trimethoxy silicane 10%, ethyl alcohol 70% and 10%.
6. the preparation method of the silicon carbide powder as described in claim 1 as organic composite material reinforcement, feature exist
In the weight ratio of the silane coupling agent and polyethyleneimine amide is 2:3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810945540.5A CN108929568A (en) | 2018-08-20 | 2018-08-20 | A kind of preparation method of the silicon carbide powder as organic composite material reinforcement |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810945540.5A CN108929568A (en) | 2018-08-20 | 2018-08-20 | A kind of preparation method of the silicon carbide powder as organic composite material reinforcement |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108929568A true CN108929568A (en) | 2018-12-04 |
Family
ID=64445989
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810945540.5A Pending CN108929568A (en) | 2018-08-20 | 2018-08-20 | A kind of preparation method of the silicon carbide powder as organic composite material reinforcement |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108929568A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112645712A (en) * | 2020-12-24 | 2021-04-13 | 西安鑫垚陶瓷复合材料有限公司 | Hydrophobic ceramic powder, carbon-ceramic composite material surface protective coating and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261409A (en) * | 2014-09-29 | 2015-01-07 | 平顶山易成新材料有限公司 | Method for preparing silicon carbide powder serving as organic composite material reinforcement |
| CN107118289A (en) * | 2017-04-25 | 2017-09-01 | 黄驰 | A kind of surface modifier of inorganic particle and preparation method thereof, application |
| CN107265469A (en) * | 2016-04-08 | 2017-10-20 | 南京唯才新能源科技有限公司 | A kind of surface modifying method of micron order aerogel powder |
-
2018
- 2018-08-20 CN CN201810945540.5A patent/CN108929568A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261409A (en) * | 2014-09-29 | 2015-01-07 | 平顶山易成新材料有限公司 | Method for preparing silicon carbide powder serving as organic composite material reinforcement |
| CN107265469A (en) * | 2016-04-08 | 2017-10-20 | 南京唯才新能源科技有限公司 | A kind of surface modifying method of micron order aerogel powder |
| CN107118289A (en) * | 2017-04-25 | 2017-09-01 | 黄驰 | A kind of surface modifier of inorganic particle and preparation method thereof, application |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112645712A (en) * | 2020-12-24 | 2021-04-13 | 西安鑫垚陶瓷复合材料有限公司 | Hydrophobic ceramic powder, carbon-ceramic composite material surface protective coating and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103146147B (en) | A kind of epoxy resin toughened/glass fibre prepreg and preparation method | |
| CN104193288A (en) | Preparation and application method of water-based ceramic anticorrosive paint | |
| CN107459774A (en) | A kind of graphene/nanometer silica/epoxy resin composite material and preparation method thereof | |
| CN105130495B (en) | A kind of high strength lightweight silica brick and preparation method thereof | |
| CN107629411A (en) | The preparation method of hollow mesoporous silica microsphere reinforced epoxy composite | |
| CN104910649A (en) | Quartz powder surface active composite modification method | |
| CN102417333A (en) | Waterproof alkali efforescence resistant slurry, waterproof alkali efforescence resistant lightweight decorative building material and production method thereof | |
| CN112226129A (en) | Antibacterial coating and preparation method thereof | |
| CN107512892A (en) | A kind of ceramic tile adhesive and preparation method thereof | |
| CN108929568A (en) | A kind of preparation method of the silicon carbide powder as organic composite material reinforcement | |
| CN107523103A (en) | A kind of aerosil coating and its application | |
| CN104028255A (en) | Magnetic surface-modified nanometer titanium dioxide and preparation method thereof | |
| CN104261409B (en) | A kind of preparation method of the silicon carbide powder as organic composite material reinforcement | |
| CN114634337A (en) | High-toughness modified aggregate inorganic artificial stone and preparation method thereof | |
| CN106519879A (en) | Preparation method of high-wear-resistance floor paint | |
| CN109836557A (en) | Toughened hydrophobic epoxy resin and preparation method thereof | |
| CN107721314B (en) | A kind of ready-mixed concrete and application thereof containing seven graded aggregates | |
| CN106221105A (en) | The photocurable resin material that a kind of anti-static type 3D prints | |
| CN111072342B (en) | Recycled aggregate pervious concrete with increased porosity and preparation method thereof | |
| CN105152659B (en) | A kind of composite silicon brick and preparation method thereof | |
| CN106495554B (en) | A kind of preparation method of stable type alkali-free quick-coagulant | |
| CN103432958B (en) | Calcium carbonate surface-active agent | |
| CN107936776A (en) | A kind of hexagonal boron nitride modified epoxy super-hydrophobic coating material and preparation method thereof | |
| CN111718152A (en) | Wormwood modified quartz stone and preparation method thereof | |
| CN109694255A (en) | A kind of microdilatancy silica brick and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181204 |
|
| RJ01 | Rejection of invention patent application after publication |