CN110527262A - Photochromic polyester fiber master batch and preparation method thereof - Google Patents

Photochromic polyester fiber master batch and preparation method thereof Download PDF

Info

Publication number
CN110527262A
CN110527262A CN201910869045.5A CN201910869045A CN110527262A CN 110527262 A CN110527262 A CN 110527262A CN 201910869045 A CN201910869045 A CN 201910869045A CN 110527262 A CN110527262 A CN 110527262A
Authority
CN
China
Prior art keywords
parts
photochromic
polyester fiber
master batch
pbt
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
Application number
CN201910869045.5A
Other languages
Chinese (zh)
Inventor
魏庭龙
刘晓峰
彭志勇
谢伟
刘向向
李珊珊
侯文杰
李林
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.)
Suzhou Baoli Di Material Polytron Technologies Inc
Original Assignee
Suzhou Baoli Di Material Polytron Technologies Inc
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 Suzhou Baoli Di Material Polytron Technologies Inc filed Critical Suzhou Baoli Di Material Polytron Technologies Inc
Priority to CN201910869045.5A priority Critical patent/CN110527262A/en
Publication of CN110527262A publication Critical patent/CN110527262A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/06Dyes
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2467/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2467/02Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention provides a kind of photochromic polyester fiber master batch, it is composed of the following components by weight: 0-90 parts of PET, 0-90 parts of PBT, 1-30 parts of photochromic powders, 0-20 parts of dyestuffs, 0.5-2.5 parts of mixtures, 0.5-1.5 parts of dispersing aiies, wherein the mixture includes heat stabilizer and antioxidant, the inherent viscosity of the PET is 0.66-0.82dL/g, and the fusing point of PET is 180-253 DEG C;The inherent viscosity of PBT is 0.82-1.0dL/g, and the fusing point of PBT is 180-230 DEG C.The present invention also provides the preparation methods of above-mentioned photochromic polyester fiber master batch.Master batch of the invention is suitable for the production of polyester fiber, and has photochromic characteristic, can solve the problems, such as existing to be made that photochromic fabric bring persistence is poor, comfort is poor, poor air permeability and environmental pollution of coating way.

Description

Photochromic polyester fiber master batch and preparation method thereof
Technical field
The present invention relates to a kind of photochromic polyester fiber master batches and preparation method thereof.
Background technique
Currently, photochromic material can be used as the ornaments such as nail varuish, carved lacquerware craftwork, T-shirt, wall paper.In order to suitable Different needs are answered, photochromic compound can be added in the auxiliary agents such as adhesive, the diluent of general ink or coating It is mixed and made into screen printing ink or coating;Photochromic material can be also made to packaging film, the dimming glass window of building, vapour Vehicle and the windscreen of aircraft etc. protect solar radiation, guarantee safety.
The photochromic fabric having in the market is obtained using the method for coating, and fabric poor air permeability, and hand are caused It is poor to feel, while bringing certain environmental pollution.In addition, being easy to fall off in washing process floating coat, color changeable effect cannot be lasting.Cause This, is badly in need of a kind of photochromic polyester fiber master batch to solve the above problems.
Summary of the invention
The purpose of the present invention is to provide a kind of photochromic polyester fiber master batch and preparation method thereof, which is applicable in In the production of polyester fiber, and there is photochromic characteristic, existing use coating way can be solved, photochromic fabric band is made The persistence come is poor, comfort is poor, poor air permeability and the problem of environmental pollution.
To achieve the above object, the present invention provides a kind of photochromic polyester fiber master batches, by weight by with The following group is grouped as:
0-90 parts of PET,
0-90 parts of PBT,
1-30 parts of photochromic powders,
0-20 parts of dyestuffs,
0.5-2.5 parts of mixtures,
0.5-1.5 parts of dispersing aiies,
Wherein, the mixture includes heat stabilizer and antioxidant, and the inherent viscosity of the PET is 0.66-0.82dL/g, and The fusing point of PET is 180-253 DEG C;The inherent viscosity of PBT is 0.82-1.0dL/g, and the fusing point of PBT is 180-230 DEG C.
Preferably, the inherent viscosity of the PET is 0.82dl/g, and the fusing point of PET is 190-230 DEG C.
Preferably, the inherent viscosity of the PBT is 1dl/g, and the fusing point of PBT is 190-230 DEG C.
Preferably, the dispersing aid is ethylene bis stearic acid amide, titanate coupling agent, silane coupling agent, silicone One or more of auxiliary agent.
Preferably, the heat stabilizer is that alkali type thermal stabilizing agent, fatty acid soap heat stabilizer, organic compound heat are steady Determine one of agent, composite type heat stabilizer, Themstab series heat stabilizer.
Preferably, the antioxidant is one or more of aromatic amine antioxidant, Hinered phenols antioxidant.
Preferably, the dyestuff is one of anthraquinone dye, heterocyclic solvent dye, methylene base class solvent dye or several Kind.
Preferably, the photochromic powder is spiro-pyrans class, diarylethene, the liquor-saturated class of fulgenic acid, discoloration microcapsules One or more of.
The present invention also provides the preparation methods of above-mentioned photochromic polyester fiber master batch, include the following steps:
1) the following raw material is taken by weight:
0-90 parts of PET,
0-90 parts of PBT,
1-30 parts of photochromic powders,
0-20 parts of dyestuffs,
0.5-2.5 parts of mixtures,
0.5-1.5 parts of dispersing aiies,
Wherein, the mixture includes heat stabilizer and antioxidant;
2) by above-mentioned raw materials PET and PBT be dried, drying temperature is 95-105 DEG C, and vacuum degree≤- 0.08MPa is dry Time is 6-12 hours, puts into batch mixer together with the other components in raw material later, mixing is sufficiently stirred;Double spiral shells are put into again Extruding pelletization in bar extruder;The material of mixing, which is sheared after being sufficiently plasticized in twin-screw through the dispersive element in twin-screw, to be dispersed Uniformly, it is drawn to pelleter through circular hole die extrusion, sink cooling, tie rod and is cut into long 3mm ± 1mm, diameter 2.5mm ± 1.5mm Cylindrical type particle;The double screw extruder is furnished with vacuum evacuation device, and the draw ratio of the double screw extruder is not less than 40: 1;Technological temperature when extrusion is 165-240 DEG C.
Preferably, in step 2, before mixing first by heat stabilizer, antioxidant, dispersing aid and photochromic powder into Row premix, and suitably heat, layer protecting film is formed on photochromic powder.
Advantages and advantages of the present invention are to provide a kind of photochromic polyester fiber master batch and its preparation side Method, which is suitable for the production of polyester fiber, and has photochromic characteristic, can solve existing use coating way and light is made Cause that color-changing face fabric bring persistence is poor, comfort is poor, poor air permeability and the problem of environmental pollution.
Specific embodiment
With reference to embodiment, the specific embodiment of the present invention is further described.Following embodiment is only used for more Add and clearly demonstrate technical solution of the present invention, and not intended to limit the protection scope of the present invention.
The technical solution that the present invention embodies is:
It is composed of the following components by weight the present invention provides a kind of photochromic polyester fiber master batch:
30 parts of PET,
40 parts of PBT,
25 parts of photochromic powders,
3 parts of dyestuffs,
1.5 parts of mixtures,
0.5 part of dispersing aid,
Wherein, the mixture is made of 1 part of heat stabilizer and 0.5 part of antioxidant, and the inherent viscosity of the PET is 0.82dL/ G, and the fusing point of PET is 180-223 DEG C;The inherent viscosity of the PBT is 1.0dL/g, and the fusing point of PBT is 180-210 DEG C; The partial size of the photochromic powder is 0.5-5.0um;The dispersing aid is ethylene bis stearic acid amide, titanate esters coupling One or more of agent, silane coupling agent, silicone analog assistant, the heat stabilizer are alkali type thermal stabilizing agent, fatty acid soaps One of type thermal stabilizing agent, organic compound heat stabilizer, composite type heat stabilizer, Themstab series heat stabilizer, The antioxidant is one or more of aromatic amine antioxidant, Hinered phenols antioxidant, and the dyestuff is anthraquinone dye, miscellaneous One or more of ring class solvent dye, methylene base class solvent dye, the photochromic powder are spiro-pyrans class, diaryl One or more of the liquor-saturated class of vinyl, fulgenic acid, discoloration microcapsules.
The present invention also provides the preparation methods of above-mentioned photochromic polyester fiber master batch, include the following steps:
1) the following raw material is taken by weight:
30 parts of PET,
40 parts of PBT,
25 parts of photochromic powders,
3 parts of anthraquinone dyes,
1.5 parts of mixtures,
0.5 part of silane coupling agent,
Wherein, the mixture is made of 1 part of heat stabilizer and 0.5 part of antioxidant;
2) by above-mentioned raw materials PET and PBT be dried, drying temperature is 95-105 DEG C, and vacuum degree≤- 0.08MPa is dry Time is 6-12 hours, then heat stabilizer, antioxidant, silane coupling agent and photochromic powder are premixed, and is suitably added Temperature forms layer protecting film on photochromic powder, puts into together with PET and PBT after anthraquinone dye and drying later In batch mixer, mixing is sufficiently stirred;Extruding pelletization in double screw extruder is put into again;The material of mixing is sufficiently moulded in twin-screw It is uniformly dispersed after change through the dispersive element shearing in twin-screw, is drawn to pelleter through circular hole die extrusion, sink cooling, tie rod It is cut into long 3mm ± 1mm, the cylindrical type particle of diameter 2.5mm ± 1.5mm;The double screw extruder is furnished with vacuum evacuation device, institute The draw ratio of double screw extruder is stated not less than 40:1;Technological temperature when extrusion is 165-240 DEG C.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications Also it should be regarded as protection scope of the present invention.

Claims (10)

1. a kind of photochromic polyester fiber master batch, which is characterized in that composed of the following components by weight:
0-90 parts of PET,
0-90 parts of PBT,
1-30 parts of photochromic powders,
0-20 parts of dyestuffs,
0.5-2.5 parts of mixtures,
0.5-1.5 parts of dispersing aiies,
Wherein, the mixture includes heat stabilizer and antioxidant, and the inherent viscosity of the PET is 0.66-0.82dL/g, and The fusing point of PET is 180-253 DEG C;The inherent viscosity of PBT is 0.82-1.0dL/g, and the fusing point of PBT is 180-230 DEG C.
2. photochromic polyester fiber master batch according to claim 1, which is characterized in that the inherent viscosity of the PET For 0.82dl/g, and the fusing point of PET is 190-230 DEG C.
3. photochromic polyester fiber master batch according to claim 2, which is characterized in that the inherent viscosity of the PBT For 1dl/g, and the fusing point of PBT is 190-230 DEG C.
4. photochromic polyester fiber master batch according to claim 3, which is characterized in that the dispersing aid is ethylene One or more of double stearic amides, titanate coupling agent, silane coupling agent, silicone analog assistant.
5. photochromic polyester fiber master batch according to claim 4, which is characterized in that the heat stabilizer is alkali Type thermal stabilizing agent, fatty acid soap heat stabilizer, organic compound heat stabilizer, composite type heat stabilizer, Themstab system One of column heat stabilizer.
6. photochromic polyester fiber master batch according to claim 5, which is characterized in that the antioxidant is aromatic amine One or more of kind antioxidant, Hinered phenols antioxidant.
7. photochromic polyester fiber master batch according to claim 6, which is characterized in that the dyestuff is anthraquinone dye One or more of material, heterocyclic solvent dye, methylene base class solvent dye.
8. photochromic polyester fiber master batch according to claim 7, which is characterized in that the photochromic powder is One or more of the liquor-saturated class of spiro-pyrans class, diarylethene, fulgenic acid, discoloration microcapsules.
9. the preparation method of photochromic polyester fiber master batch described in any one of claims 1 to 8, which is characterized in that packet Include following steps:
1) the following raw material is taken by weight:
0-90 parts of PET,
0-90 parts of PBT,
1-30 parts of photochromic powders,
0-20 parts of dyestuffs,
0.5-2.5 parts of mixtures,
0.5-1.5 parts of dispersing aiies,
Wherein, the mixture includes heat stabilizer and antioxidant;
2) by above-mentioned raw materials PET and PBT be dried, drying temperature is 95-105 DEG C, and vacuum degree≤- 0.08MPa is dry Time is 6-12 hours, puts into batch mixer together with the other components in raw material later, mixing is sufficiently stirred;Double spiral shells are put into again Extruding pelletization in bar extruder;The material of mixing, which is sheared after being sufficiently plasticized in twin-screw through the dispersive element in twin-screw, to be dispersed Uniformly, it is drawn to pelleter through circular hole die extrusion, sink cooling, tie rod and is cut into long 3mm ± 1mm, diameter 2.5mm ± 1.5mm Cylindrical type particle;The double screw extruder is furnished with vacuum evacuation device, and the draw ratio of the double screw extruder is not less than 40: 1;Technological temperature when extrusion is 165-240 DEG C.
10. the preparation method of photochromic polyester fiber master batch according to claim 9, which is characterized in that in step 2) in, first heat stabilizer, antioxidant, dispersing aid and photochromic powder are premixed before mixing, and suitably heats, in light Layer protecting film is formed on mutagens toner body.
CN201910869045.5A 2019-09-16 2019-09-16 Photochromic polyester fiber master batch and preparation method thereof Pending CN110527262A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910869045.5A CN110527262A (en) 2019-09-16 2019-09-16 Photochromic polyester fiber master batch and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910869045.5A CN110527262A (en) 2019-09-16 2019-09-16 Photochromic polyester fiber master batch and preparation method thereof

Publications (1)

Publication Number Publication Date
CN110527262A true CN110527262A (en) 2019-12-03

Family

ID=68668715

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910869045.5A Pending CN110527262A (en) 2019-09-16 2019-09-16 Photochromic polyester fiber master batch and preparation method thereof

Country Status (1)

Country Link
CN (1) CN110527262A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110591303A (en) * 2019-09-20 2019-12-20 苏州宝丽迪材料科技股份有限公司 Photochromic color master batch for skin-core structure fiber core layer and preparation method thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103436178A (en) * 2013-09-04 2013-12-11 广西大学 Long-term storage method of rosin pentaerythritol ester
CN104817827A (en) * 2015-04-17 2015-08-05 苏州宝力塑胶材料有限公司 Terylene colorful fiber master batch with ultraviolet protection function and preparation method thereof
CN106189123A (en) * 2016-08-29 2016-12-07 佛山市高明区尚润盈科技有限公司 A kind of preparation method of photochromic PET/PTT alloy
CN106519415A (en) * 2016-11-16 2017-03-22 广东顺德鲁华光电新材料实业有限公司 Flame-retardant plastic with photochromic and antistatic functions and preparation method thereof
CN106700439A (en) * 2016-12-13 2017-05-24 苏州宝力塑胶材料有限公司 Flat polyester fiber master batch applicable to spun dyeing process and preparation method of master batch
CN106947204A (en) * 2017-04-11 2017-07-14 华南协同创新研究院 3D printing reversible sensitization discoloration PHA composites and its preparation method and purposes
CN110128798A (en) * 2019-05-23 2019-08-16 浙江金彩新材料有限公司 A kind of terylene light becomes master batch and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103436178A (en) * 2013-09-04 2013-12-11 广西大学 Long-term storage method of rosin pentaerythritol ester
CN104817827A (en) * 2015-04-17 2015-08-05 苏州宝力塑胶材料有限公司 Terylene colorful fiber master batch with ultraviolet protection function and preparation method thereof
CN106189123A (en) * 2016-08-29 2016-12-07 佛山市高明区尚润盈科技有限公司 A kind of preparation method of photochromic PET/PTT alloy
CN106519415A (en) * 2016-11-16 2017-03-22 广东顺德鲁华光电新材料实业有限公司 Flame-retardant plastic with photochromic and antistatic functions and preparation method thereof
CN106700439A (en) * 2016-12-13 2017-05-24 苏州宝力塑胶材料有限公司 Flat polyester fiber master batch applicable to spun dyeing process and preparation method of master batch
CN106947204A (en) * 2017-04-11 2017-07-14 华南协同创新研究院 3D printing reversible sensitization discoloration PHA composites and its preparation method and purposes
CN110128798A (en) * 2019-05-23 2019-08-16 浙江金彩新材料有限公司 A kind of terylene light becomes master batch and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110591303A (en) * 2019-09-20 2019-12-20 苏州宝丽迪材料科技股份有限公司 Photochromic color master batch for skin-core structure fiber core layer and preparation method thereof

Similar Documents

Publication Publication Date Title
CN101392077B (en) Polypropylene color master-batch with pearlescent interference effect and preparation method thereof
EP1509577B1 (en) Carbon black and compositions containing same
ITMI20070089A1 (en) GRAIN OF THERMOPLASTIC POLYMER AND / OR COLORED THERMO-HARDENER AND / OR ADDITIVATE AND RELATIVE PROCEDURE OF COLORING AND / OR ADDITIVATION
JP6822784B2 (en) Dimming composition for 3D printing
JP4014691B2 (en) Bismuth vanadate pigment powder mixture
DE69421314T2 (en) Process for the production of colored thermoplastic resin pellets
CN110527262A (en) Photochromic polyester fiber master batch and preparation method thereof
CN106700439A (en) Flat polyester fiber master batch applicable to spun dyeing process and preparation method of master batch
CN110607059A (en) Photochromic polylactic acid fiber master batch and preparation method thereof
CN110615931A (en) Temperature-sensitive color-changing stationery case and preparation method thereof
CN110591303A (en) Photochromic color master batch for skin-core structure fiber core layer and preparation method thereof
CN108865052A (en) Single-component dealcoholization-type silicone structure sealant of building curtain wall and preparation method thereof
CN1594600A (en) Leather with variable surface color and manufacturing process thereof
CN108192240B (en) Photochromic PVC heat-shrinkable label film and preparation method thereof
JPS5898456A (en) Production of fabrics
CN110041759A (en) Photonic crystal ink and its printing process and printed matter
JPH06345879A (en) Ultraviolet light-blocking film and ultraviolet light-blocking container
US3316205A (en) Colored plastic compositions and colors therefor
CN108659743A (en) A kind of environment-friendly type glue spraying and preparation method thereof
JPH07224228A (en) Colored polymer composition
CN106543661A (en) A kind of preparation method of Novel color-changing 3D printing material
US2998402A (en) Process for dyeing and coloring in the mass with perlyene derivatives
NL1013644C2 (en) Laser-markable polymer composition.
CN111303458A (en) Preparation method of light-resistant and antibacterial color master batch
JPH05222303A (en) Method for mass coloration of plastic

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: 20191203

RJ01 Rejection of invention patent application after publication