CN103741517A - Printing paste used for gold powder printing of stone wall paper and preparation method - Google Patents
Printing paste used for gold powder printing of stone wall paper and preparation method Download PDFInfo
- Publication number
- CN103741517A CN103741517A CN201310743257.1A CN201310743257A CN103741517A CN 103741517 A CN103741517 A CN 103741517A CN 201310743257 A CN201310743257 A CN 201310743257A CN 103741517 A CN103741517 A CN 103741517A
- Authority
- CN
- China
- Prior art keywords
- parts
- mass
- printing
- acrylic acid
- rheological agent
- 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.)
- Granted
Links
Landscapes
- Inks, Pencil-Leads, Or Crayons (AREA)
- Paints Or Removers (AREA)
- Paper (AREA)
Abstract
The invention discloses printing paste used for gold powder printing of stone wall paper and a preparation method. The printing paste is prepared by carrying out the following steps: emulsifying 2.0-2.2 parts by mass of 1,4-butanediol dimethacrylate, 1.0-1.1 parts by mass of itaconic acid, 130-140 parts by mass of ethyl acrylate, 31-32 parts by mass of butyl acrylate, 6.4-6.6 parts by mass of hydroxyethyl methylacrylate, 27-28 parts by mass of methyl methacrylate, 4.0-4.2 parts by mass of 2-(methacryloyloxy)ethyl acetoacetate, 32-33 parts by mass of styrene, 2-2.3 parts by mass of fatty alcohol-polyoxyethylene ether 23E9 and 230-250 parts by mass of deionized water, and initiating polymerization; compounding 20-25 parts by mass of a mixed solution of sorbitol and benzotriazole, 20-22 parts by mass of an associative leveling rheological agent and 10-15 parts by mass of an acrylic dispersant, and mixing. The printing paste in high in transparency, glossiness and fastness, and is resistant to air oxidation.
Description
Technical field
What the present invention relates to is a kind of stone wallpaper gold printing printing paste, the printing paste using for the color patterned pattern of stone wallpaper bronze printing.
Background technology
Stone wallpaper is take calcium carbonate as main raw material, and macromolecular material and multiple inorganic matter are that auxiliary material is made.
Prior art does not have the special printing paste of stone wallpaper, all with adhesive, replaces printing paste to use, and as the adhesives I T with BASF, adds thickener, water, print paste to mix, and does stone wallpaper printing paste and uses.Pattern glossiness, elasticity, the feel printed do not comply with one's wishes, and concave-convex sense is not strong.Particularly during gold printing, above-mentioned shortcoming is more obvious, and resistance to air oxygen voltinism is bad, easily loses the magnificent gloss of bronze.
Stone wallpaper gold printing printing paste, is not shown at present and has special product and technology openly.
Summary of the invention
The object of this invention is to provide a kind of stone wallpaper gold printing printing paste and preparation method,
This printing paste adds bronze to carry out stamp, has bronze good dispersion, and gold printing transparency, glossiness, fastness are good, and concave-convex sense is strong, and feel is soft, and the magnificent gloss retentivity of the bronze of resistance to air oxidation is good.And product processes is simple.
The present invention
stone wallpaper gold printing printing paste;
Raw material weight ratio:
Dimethacrylate 1.4 butanediol ester 2.0-2.2, itaconic acid 1.0-1.1, ethyl acrylate 130-140, butyl acrylate 31-32, hydroxyethyl methylacrylate 6.4-6.6, methyl methacrylate 27-28, acetoacetoxyethyl methacrylate 4.0-4.2, styrene 32-33, fatty alcohol-polyoxyethylene ether 23E9 are 2-2.3, deionized water 230-250, after Over emulsfication, initiated polymerization, mixed liquor 20-25, the association type levelling rheological agent 20-22 of composite sorbierite and phenylpropyl alcohol triazole, acrylic acid dispersant 10-15, mixing makes;
Product chemical index is as follows:
Outward appearance: oyster white thick liquid
Ionic: the moon
PH value: 7 ± 0.5
Solid content: >=50%.
Association type levelling rheological agent: be the product association type levelling rheological agent WT-203 of the modest Shanghai of DS Chemical Co., Ltd..
Acrylic acid dispersant: be Henkel chemical company product acrylic acid dispersant 5040.
Stone wallpaper gold printing printing paste preparation method of the present invention:
Raw material is by weight ratio:
(1) emulsification mix monomer: adding dimethacrylate 1.4 butanediol ester 2.0-2.2, itaconic acid 1.0-1.1, ethyl acrylate 130-140, butyl acrylate 31-32, hydroxyethyl methylacrylate 6.4-6.6, methyl methacrylate 27-28, acetoacetoxyethyl methacrylate 4.0-4.2, styrene 32-33, fatty alcohol-polyoxyethylene ether 23E9 in stainless steel still is 2-2.3, deionized water 210-230, emulsion is made in stirring, stand-by;
(2) initiated polymerization: get 30% of above-mentioned emulsion gross weight and add in reactor, be warming up to 80-82 ℃, add the mixed liquor of initiator ammonium persulfate 1.27 and deionized water 10, cause, then at 80-82 ℃ of temperature, drip remaining emulsion, drip ammonium persulfate 0.63-0.83 and deionized water 10 mixed liquors simultaneously, within 1-2 hour, dropwise, at 80-82 ℃ of insulation 2-3 hour, be then cooled to 30-40 ℃, with mass percent concentration, be that 20% ammoniacal liquor adjust pH is 7 ± 0.5;
(3) composite: sorbierite and phenylpropyl alcohol triazole are added in above-mentioned polymer and stirred by 1:1 mixed dissolution liquid 20-25, add acrylic acid dispersant 10-15 to stir, then add association type levelling rheological agent 20-22, stirring thickening is even, filter discharging, obtain stone wallpaper gold printing printing paste.
Association type levelling rheological agent: be the product association type levelling rheological agent WT-203 of the modest Shanghai of DS Chemical Co., Ltd..
Acrylic acid dispersant: be Henkel chemical company product acrylic acid dispersant 5040.
Product using method of the present invention:
Getting the said goods adds bronze 15% to stir to obtain gold printing slurry.
Stamp bronze is copper bronze, is divided into blue or green bronze, red bronze, gold powder etc. on color and luster.Copper bronze fineness can be carried out choice for use as required.
The present invention selects methacrylic acid 1.4 butanediol esters, itaconic acid, ethyl acrylate, butyl acrylate, hydroxyethyl methylacrylate, methyl methacrylate, acetoacetoxyethyl methacrylate, styrene monomer copolymerization.
Wherein methyl methacrylate monomer vitrification point is high, can make clarity in polymers strong, and gloss is high.Methacrylic acid 1.4 butanediol esters, hydroxyethyl methylacrylate are used in conjunction with, and can make polymerizate crosslinked between linear macromolecule, make it to form network structure, can make polymerizate have very strong crosslinked ability.Acetoacetoxyethyl methacrylate, is more suitable for height admittedly synthetic containing acrylic emulsions, can make polymer film formation at low temp good, and have outstanding elasticity and weatherability, makes polymer film forming continuous, soft.
In composite, add acrylic acid dispersant 5040 can make polymer adding in bronze process, more easily disperse, make the more even of powdery bronze dispersion, thereby make the pattern of printing more plentiful beautiful.Antioxidant phenylpropyl alcohol triazole, in gold printing, antioxidant effect is best, the special corrosion inhibitor that it is copper, can produce insoluble mixture with copper, can prevent bronze oxidation stain in air, therefore the wallpaper of gained is starched with gold printing, transparency is good, glossiness is high, fastness is good, and feel is soft, adds bronze easily to disperse, resistance to air oxidation, the gloss that Long contact time air bronze is magnificent is unaffected.
The specific embodiment
Embodiment 1
Raw material weight ratio:
(1) emulsification mix monomer: adding 2.0 parts of dimethacrylate 1.4 butanediol esters, 1.0 parts of itaconic acids, 130 parts of ethyl acrylates, 31 parts of butyl acrylates, 6.4 parts of hydroxyethyl methylacrylates, 27 parts of methyl methacrylates, 4.0 parts of acetoacetoxyethyl methacrylate, 32 parts of styrene, fatty alcohol-polyoxyethylene ether 23E9 in stainless steel still is 210 parts of 2 parts, deionized water, emulsion is made in stirring, stand-by;
(2) initiated polymerization: get 30% of above-mentioned emulsion gross weight and add in reactor, be warming up to 80-82 ℃, add the mixed liquor of 1.27 parts of initiator ammonium persulfates and 10 parts of deionized waters, cause, then at 80-82 ℃ of temperature, drip remaining emulsion, drip 0.63 part of ammonium persulfate and 10 portions of mixed liquors of deionized water simultaneously, within 1 hour, dropwise, at 80-82 ℃ of insulation 2-3 hour, be then cooled to 30-40 ℃, with mass percent concentration, be that 20% ammoniacal liquor adjust pH is 7 ± 0.5;
(3) composite: 10 parts of sorbierites are added in polymer and stirred with 10 parts of mixed dissolution liquid of phenylpropyl alcohol triazole, add 10 parts of stirrings of acrylic acid dispersant, then add 20 parts of association type levelling rheological agents, stir, filter discharging, obtain stone wallpaper gold printing printing paste.
Embodiment 2
(1) emulsification mix monomer: adding 2.1 parts of dimethacrylate 1.4 butanediol esters, 1.05 parts of itaconic acids, 135 parts of ethyl acrylates, 31.5 parts of butyl acrylates, 6.5 parts of hydroxyethyl methylacrylates, 27.5 parts of methyl methacrylates, 4.1 parts of acetoacetoxyethyl methacrylate, 32.5 parts of styrene, fatty alcohol-polyoxyethylene ether 23E9 in stainless steel still is 220 parts of 2.2 parts, deionized water, emulsion is made in stirring, stand-by;
(2) initiated polymerization: get 30% of above-mentioned emulsion gross weight and add in reactor, be warming up to 80-82 ℃, add the mixed liquor of 1.27 parts of initiator ammonium persulfates and 10 parts of deionized waters, cause, then at 80-82 ℃ of temperature, drip remaining emulsion, drip 0.73 part of ammonium persulfate and 10 portions of mixed liquors of deionized water simultaneously, within 1.5 hours, dropwise, at 80-82 ℃ of insulation 2-3 hour, then being cooled to 30-40 ℃, is that 20% ammoniacal liquor adjust pH is 7 ± 0.5 with mass percent concentration;
(3) composite: 12 parts of sorbierites are added in polymer and stirred with 12 parts of mixed dissolution liquid of phenylpropyl alcohol triazole, add 12.5 parts of stirrings of acrylic acid dispersant, then add 21 parts of association type levelling rheological agents, stirring thickening is even, filter discharging, obtain stone wallpaper gold printing printing paste.
Embodiment 3
(1) emulsification mix monomer: adding 2.2 parts of dimethacrylate 1.4 butanediol esters, 1.1 parts of itaconic acids, 140 parts of ethyl acrylates, 32 parts of butyl acrylates, 6.6 parts of hydroxyethyl methylacrylates, 28 parts of methyl methacrylates, 4.2 parts of acetoacetoxyethyl methacrylate, 33 parts of styrene, fatty alcohol-polyoxyethylene ether 23E9 in stainless steel still is 230 parts of 2.3 parts, deionized water, emulsion is made in stirring, stand-by;
(2) initiated polymerization: get 30% of above-mentioned emulsion gross weight and add in reactor, be warming up to 80-82 ℃, add the mixed liquor of 1.27 parts of initiator ammonium persulfates and 10 parts of deionized waters, cause, then at 80-82 ℃ of temperature, drip remaining emulsion, drip 0.83 part of ammonium persulfate and 10 portions of mixed liquors of deionized water simultaneously, within 2 hours, dropwise, at 80-82 ℃ of insulation 2-3 hour, be then cooled to 30-40 ℃, with mass percent concentration, be that 20% ammoniacal liquor adjust pH is 7 ± 0.5;
(3) composite: 12.5 parts of sorbierites are added in polymer and stirred with 12.5 parts of mixed dissolution liquid of phenylpropyl alcohol triazole, add 15 parts of stirrings of acrylic acid dispersant, then add 22 grams of association type levelling rheological agents, stirring thickening is even, filter discharging, obtain stone wallpaper gold printing printing paste.
Association type levelling rheological agent described in above-described embodiment: be the product association type levelling rheological agent WT-203 of the modest Shanghai of DS Chemical Co., Ltd..
Acrylic acid dispersant described in above-described embodiment: be Henkel chemical company product acrylic acid dispersant 5040.
Experimental example:
Get embodiment of the present invention 1-3 product, add respectively the bronze of 15% weight to stir, obtain stone wallpaper gold printing slurry.
Adopt rotary screen printing machines stamp on stone paper wallpaper, dry 3 minutes for 70-80 ℃.
After experimental example product and printing, testing result is as follows:
| Project | Experimental example 1 | Experimental example 2 | Experimental example 3 |
| Fine and smooth degree | Fine and smooth | Fine and smooth | Fine and smooth |
| Transparency | Good | Good | Good |
| Glossiness | Magnificent gloss | Magnificent gloss | Magnificent gloss |
| Oxidative resistance | Nondiscolouring | Nondiscolouring | Nondiscolouring |
| Feel elasticity | Soft good springiness | Soft good springiness | Soft good springiness |
| Dispersed | Easily disperse | Easily disperse | Easily disperse |
| Dry fastness | 5 grades | 5 grades | 5 grades |
| Fastness to wet rubbing | 5 grades | 5 grades | 5 grades |
Dry fastness to wet rubbing test is pressed GB/3920 and is carried out.
Sophistication, glossiness ocular estimate.
Oxidative resistance adopts the test of solarization climate test instrument: be divided into nondiscolouring, light discolouration, serious discoloration.
Feel, elasticity hand touching test.
Uniformity coefficient test after dispersed employing range estimation adds bronze to stir.
Known by above result, this product is applied on environment-friendly type stone wallpaper has that transparency is good, glossiness is high, fastness good, feel is soft, add bronze easily to disperse, resistance to air oxidation, the gloss that Long contact time air bronze is magnificent is unaffected, production technology is simple, and meets the feature of environmental requirement.
Claims (4)
1. stone wallpaper gold printing printing paste, is characterized in that;
Raw material weight ratio:
Dimethacrylate 1.4 butanediol ester 2.0-2.2, itaconic acid 1.0-1.1, ethyl acrylate 130-140, butyl acrylate 31-32, hydroxyethyl methylacrylate 6.4-6.6, methyl methacrylate 27-28, acetoacetoxyethyl methacrylate 4.0-4.2, styrene 32-33, fatty alcohol-polyoxyethylene ether 23E9 are 2-2.3, deionized water 230-250, after Over emulsfication, initiated polymerization, mixed liquor 20-25, the association type levelling rheological agent 20-22 of composite sorbierite and phenylpropyl alcohol triazole, acrylic acid dispersant 10-15, mixing makes;
Product chemical index is as follows:
Outward appearance: oyster white thick liquid
Ionic: the moon
PH value: 7 ± 0.5
Solid content: >=50%;
Association type levelling rheological agent: be the product association type levelling rheological agent WT-203 of the modest Shanghai of DS Chemical Co., Ltd.;
Acrylic acid dispersant: be Henkel chemical company product acrylic acid dispersant 5040.
2. the preparation method of gold printing slurry for stone wallpaper, is characterized in that:
Raw material is by weight ratio:
(1) emulsification mix monomer: adding dimethacrylate 1.4 butanediol ester 2.0-2.2, itaconic acid 1.0-1.1, ethyl acrylate 130-140, butyl acrylate 31-32, hydroxyethyl methylacrylate 6.4-6.6, methyl methacrylate 27-28, acetoacetoxyethyl methacrylate 4.0-4.2, styrene 32-33, fatty alcohol-polyoxyethylene ether 23E9 in stainless steel still is 2-2.3, deionized water 210-230, emulsion is made in stirring, stand-by;
(2) initiated polymerization: get 30% of above-mentioned emulsion gross weight and add in reactor, be warming up to 80-82 ℃, add the mixed liquor of initiator ammonium persulfate 1.27 and deionized water 10, cause, then at 80-82 ℃ of temperature, drip remaining emulsion, drip ammonium persulfate 0.63-0.83 and deionized water 10 mixed liquors simultaneously, within 1-2 hour, dropwise, at 80-82 ℃ of insulation 2-3 hour, be then cooled to 30-40 ℃, with mass percent concentration, be that 20% ammoniacal liquor adjust pH is 7 ± 0.5;
(3) composite: sorbierite and phenylpropyl alcohol triazole are added in above-mentioned polymer and stirred by 1:1 mixed dissolution liquid 20-25, add acrylic acid dispersant 10-15 to stir, then add association type levelling rheological agent 20-22, stirring thickening is even, filter discharging, obtain stone wallpaper gold printing printing paste.
3. the preparation method of gold printing slurry for stone wallpaper according to claim 2, is characterized in that:
Association type levelling rheological agent is the product association type levelling rheological agent WT-203 of the modest Shanghai of DS Chemical Co., Ltd.;
Acrylic acid dispersant is Henkel chemical company product acrylic acid dispersant 5040.
4. the stone wallpaper gold printing printing paste obtaining as claim 2 method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310743257.1A CN103741517B (en) | 2013-12-30 | 2013-12-30 | Stone wallpaper gold printing printing paste and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310743257.1A CN103741517B (en) | 2013-12-30 | 2013-12-30 | Stone wallpaper gold printing printing paste and preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103741517A true CN103741517A (en) | 2014-04-23 |
| CN103741517B CN103741517B (en) | 2015-10-28 |
Family
ID=50498577
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310743257.1A Active CN103741517B (en) | 2013-12-30 | 2013-12-30 | Stone wallpaper gold printing printing paste and preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103741517B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965395A (en) * | 2014-05-21 | 2014-08-06 | 辽宁恒星精细化工有限公司 | Modified acrylate foam coating emulsion and preparation method thereof |
| CN110904701A (en) * | 2019-12-17 | 2020-03-24 | 辽宁恒星精细化工有限公司 | Printing paste for polyvinyl chloride material handicraft leaves and preparation method thereof |
| CN112694561A (en) * | 2020-12-23 | 2021-04-23 | 辽宁恒星精细化工有限公司 | Preparation method and application of water-based acrylate adhesive cement |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6331598B1 (en) * | 1998-08-25 | 2001-12-18 | Korea Chemical Co., Ltd. | Emulsion polymer having a vesiculated structure and the process for preparing the same |
| JP2009084709A (en) * | 2007-09-27 | 2009-04-23 | Chuo Rika Kogyo Corp | Aqueous resin dispersion for textile processing |
| CN101942771A (en) * | 2010-08-17 | 2011-01-12 | 辽宁恒星精细化工有限公司 | Cotton-polyester fabric burn-out printing gum and preparation method thereof |
| CN102619102A (en) * | 2012-04-06 | 2012-08-01 | 辽宁恒星精细化工有限公司 | Embossed printing paste for velvet fabric and preparation method thereof |
| CN103088674A (en) * | 2012-12-26 | 2013-05-08 | 辽宁恒星精细化工有限公司 | Bright film printing paste and preparation method thereof |
-
2013
- 2013-12-30 CN CN201310743257.1A patent/CN103741517B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6331598B1 (en) * | 1998-08-25 | 2001-12-18 | Korea Chemical Co., Ltd. | Emulsion polymer having a vesiculated structure and the process for preparing the same |
| JP2009084709A (en) * | 2007-09-27 | 2009-04-23 | Chuo Rika Kogyo Corp | Aqueous resin dispersion for textile processing |
| CN101942771A (en) * | 2010-08-17 | 2011-01-12 | 辽宁恒星精细化工有限公司 | Cotton-polyester fabric burn-out printing gum and preparation method thereof |
| CN102619102A (en) * | 2012-04-06 | 2012-08-01 | 辽宁恒星精细化工有限公司 | Embossed printing paste for velvet fabric and preparation method thereof |
| CN103088674A (en) * | 2012-12-26 | 2013-05-08 | 辽宁恒星精细化工有限公司 | Bright film printing paste and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965395A (en) * | 2014-05-21 | 2014-08-06 | 辽宁恒星精细化工有限公司 | Modified acrylate foam coating emulsion and preparation method thereof |
| CN103965395B (en) * | 2014-05-21 | 2016-01-13 | 辽宁恒星精细化工有限公司 | Modification acrylate intumescent coating emulsion and preparation method |
| CN110904701A (en) * | 2019-12-17 | 2020-03-24 | 辽宁恒星精细化工有限公司 | Printing paste for polyvinyl chloride material handicraft leaves and preparation method thereof |
| CN110904701B (en) * | 2019-12-17 | 2022-02-01 | 辽宁恒星精细化工有限公司 | Printing paste for polyvinyl chloride material handicraft leaves and preparation method thereof |
| CN112694561A (en) * | 2020-12-23 | 2021-04-23 | 辽宁恒星精细化工有限公司 | Preparation method and application of water-based acrylate adhesive cement |
| CN112694561B (en) * | 2020-12-23 | 2022-07-26 | 辽宁恒星精细化工有限公司 | Preparation method and application of water-based acrylate adhesive cement |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103741517B (en) | 2015-10-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107266626B (en) | A kind of multiple self-crosslinking core-shell type lotion of room temperature and its preparation method and application | |
| CN102558427B (en) | Polymer emulsion for water-based printing ink and preparation method thereof | |
| JPH0627155B2 (en) | Emulsion copolymer containing alkyl acrylamide for thickening | |
| EP0013836A1 (en) | Compositions containing acrylic emulsion copolymers and their use as thickeners | |
| IE57180B1 (en) | Crotonate-containing copolymers,processes for their preparation and their use as thickeners in aqueous systems and as sizing agents | |
| CN105255298B (en) | A kind of true mineral varnish emulsion of vinegar phenylpropyl alcohol and preparation method | |
| CN102146247B (en) | Waterproof coating containing polyether-modified silicon-acrylic soft resin and preparation method thereof | |
| CN103756601B (en) | Metal(lic)powder tackiness agent and preparation method thereof and wallpaper, textiles | |
| DE1570312A1 (en) | Process for the preparation of polymer dispersions | |
| CN107805437A (en) | It is a kind of to be used to repair aqueous woodware paint of color and preparation method thereof | |
| CN103088674B (en) | Bright film printing paste and preparation method thereof | |
| CN103741517B (en) | Stone wallpaper gold printing printing paste and preparation method | |
| CN105524225A (en) | Core-shell type polyacrylate emulsion printing adhesive | |
| CN101457499A (en) | Surface sizing agent and its production method | |
| CN104151920A (en) | Water-based polishing printing ink for online polishing printing and preparation method | |
| CN105884962B (en) | A kind of lacquer lotion and using the lotion as the lacquer of film forming matter | |
| CN103254370A (en) | Water-based pre-printing emulsion and preparation method thereof | |
| CN103910859A (en) | Novel alkyd resin and preparation method thereof | |
| CN101581045B (en) | Elastic colorized printing paste and production method thereof | |
| CN110527011A (en) | A kind of water polyacrylic acid emulsion resin and the preparation method and application thereof | |
| CN106750039B (en) | A kind of rosin/acrylate nuclear-shell emulsion and the preparation method and application thereof | |
| JPH05295048A (en) | Aqueous resin composition | |
| CN103265659B (en) | Polyvinyl acetate/polystyrene composite emulsion with high covering power polyvinyl and preparation method thereof | |
| CN104086686A (en) | Styrene-acrylic emulsion with excellent freeze-thaw stability as well as preparation method and application thereof | |
| CN104693340A (en) | Carpentry paint emulsion with core-shell structure and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |