CN107216432B - A kind of preparation method of pressure sensitive adhesive for ultrathin double-face glue - Google Patents
A kind of preparation method of pressure sensitive adhesive for ultrathin double-face glue Download PDFInfo
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- CN107216432B CN107216432B CN201710501176.9A CN201710501176A CN107216432B CN 107216432 B CN107216432 B CN 107216432B CN 201710501176 A CN201710501176 A CN 201710501176A CN 107216432 B CN107216432 B CN 107216432B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F293/00—Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/62—Monocarboxylic acids having ten or more carbon atoms; Derivatives thereof
- C08F220/68—Esters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J153/00—Adhesives based on block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
Abstract
The invention discloses a kind of preparation method of the pressure sensitive adhesive for ultrathin double-face glue, include the following steps：（1）Raw material weigh it is spare,（2）It is prepared by finished product reaction.The present invention has carried out special improvement to the manufacture craft of pressure sensitive adhesive and has handled, and effectively improves overall high temperature resistant bonding performance, and simple production process, and the market competitiveness is high.
Description
Technical field
The invention belongs to double faced adhesive tape to fabricate field, and in particular to a kind of preparation of pressure sensitive adhesive for ultrathin double-face glue
Method.
Background technology
Double faced adhesive tape is to show one of article common in people's daily life, it is in fields such as packaging, Electronic products manufacturings
In be widely used.PET double faced adhesive tapes are one of categories common in double faced adhesive tape, and PET double faced adhesive tapes on the market use mostly at present
Traditional acrylic acid solvent-borne type glue is made, and thickness is mostly 30 ~ 50um, if the coating for reducing acrylic acid solvent-borne type glue is thick
Degree, adhesion also decline therewith.The more preferable pressure sensitive adhesive of performance is attempted to this people to be improved as adhesive, and is obtained
Good using effect, as Application No. 201410371874.8 discloses a kind of pressure sensitive adhesive applied to ultrathin double-face glue,
It is mainly mixed and modified to acrylate progress using terpene phenol resin, finally effectively improves the adhesion of double faced adhesive tape, and have
There is certain resistance to temp effect, use value is preferable.And found during long-term use, when environment temperature reaches a certain level
When, the adhesive properties of above-mentioned double faced adhesive tape substantially reduce, and the terpene phenol resin of addition can slowly migrate formation to copolymer surface
Three-phase resin bed, and then overall bonding strength is have impact on, resistance to temp effect still has to be hoisted.
The content of the invention
The purpose of the present invention is for it is existing the problem of, there is provided a kind of preparation side of pressure sensitive adhesive for ultrathin double-face glue
Method.
The present invention is achieved by the following technical solutions：
A kind of preparation method of pressure sensitive adhesive for ultrathin double-face glue, includes the following steps：
（1）Raw material weighs spare：
It is spare that following material is weighed by corresponding parts by weight：40 ~ 45 parts of butyl acrylates, 15 ~ 20 parts of acrylic acid 2- ethyl hexyls
Ester, 3 ~ 4 parts of hydroxy-ethyl acrylates, 1 ~ 3 part of dioctyl phthalate, 73 ~ 77 parts of toluene, 55 ~ 60 parts of ethyl acetate, 1 ~ 2 part
Benzoyl peroxide, 2.5 ~ 3.5 parts of dilauroyl peroxides, 25 ~ 35 parts of terpene phenol resins, 0.5 ~ 1.5 part of aluminium acetylacetonate,
0.1 ~ 0.2 part of cerium oxide, 5 ~ 10 parts of octadecyl acrylates；
（2）It is prepared by finished product reaction：
A. first by step（1）The ethyl acetate weighed is divided into two parts, and benzoyl peroxide is equally divided into two
Divide spare；
B. by operate a divide a part of ethyl acetate, a part of benzoyl peroxide mixing be put into reaction kettle, at the same time
Butyl acrylate, 2-EHA, hydroxy-ethyl acrylate, dioctyl phthalate and toluene are added, heating is not
It is spare after 35 ~ 45min of disconnected stir process；
C. another part ethyl acetate and another part benzoyl peroxide are added into the reaction kettle after operation b processing,
Dilauroyl peroxide, terpene phenol resin, aluminium acetylacetonate, cerium oxide and octadecyl acrylate are added at the same time, and heating is not
Take out spare after disconnected 1 ~ 1.2h of stir process, air is during which constantly passed through into reaction kettle；
D. the mixture for operating gained after c is handled is taken out, after eliminating its interior residual bubbles with ultrasonic wave, is cooled to room
Temperature gets product pressure sensitive adhesive.
Further, step（2）The heating and temperature control operated described in b is 75 ~ 80 DEG C, and the speed control of stirring is
350 ~ 400 revs/min.
Further, step（2）The heating and temperature control operated described in c is 85 ~ 90 DEG C, and the speed control of stirring is
500 ~ 550 revs/min.
Further, step（2）The application frequency for operating the ultrasonic wave described in d is 58 ~ 62kHz.
More to the modification processing method of polyacrylate dispersion class adhesive, the effect of the corresponding enhancing of different processing is not
Together, as Application No. 201410371874.8 is disclosed in a kind of pressure sensitive adhesive applied to ultrathin double-face glue, terpenes is mainly utilized
Phenol resin carries out acrylate mixed and modified so that its room temperature adhesion greatly promotes, and holds glutinous effect under higher temperature
It is remarkably reinforced, but when the environment temperature higher used（More than 80 DEG C）When can find that the adhesive properties of pressure sensitive adhesive decline to a great extent, this
Goal of the invention is to further lift its heatproof adhesive properties, improvement processing has been carried out to its preparation method, wherein in raw material
Selection with the addition of cerium oxide and octadecyl acrylate in component, in preparation manipulation c, constantly in the reactant into reaction kettle
Air is passed through, under conditions of high temperature and higher oxygen content, cerium oxide can be catalyzed the surface energy for strengthening a variety of reactant components, promote
Into Raolical polymerizable, the more complicated starblock acrylate copolymer of a kind of more highly branched chain, structure is formed, by terpene phenolic
The components such as resin are directly participated in polymerisation, are conducive to be lifted the chemical bonding between acrylate and terpene phenol resin and are imitated
Fruit, the octadecyl acrylate of addition are incorporated into the main chain of polymer, can lift the compatible knot of polymer and low surface energy substrates
Conjunction property, plays good increasing stick effect.
The present invention has the following advantages compared with prior art：
The present invention has carried out special improvement to the manufacture craft of pressure sensitive adhesive and has handled, and effectively improves overall high temperature resistant and glues
Performance, and simple production process are tied, the market competitiveness is high.
Embodiment
Embodiment 1
A kind of preparation method of pressure sensitive adhesive for ultrathin double-face glue, includes the following steps：
（1）Raw material weighs spare：
It is spare that following material is weighed by corresponding parts by weight：40 parts of butyl acrylates, 15 parts of 2-EHAs, 3 parts
Hydroxy-ethyl acrylate, 1 part of dioctyl phthalate, 73 parts of toluene, 55 parts of ethyl acetate, 1 part of benzoyl peroxide, 2.5 parts
Dilauroyl peroxide, 25 parts of terpene phenol resins, 0.5 part of aluminium acetylacetonate, 0.1 part of cerium oxide, 5 parts of octadecyl acrylates；
（2）It is prepared by finished product reaction：
A. first by step（1）The ethyl acetate weighed is divided into two parts, and benzoyl peroxide is equally divided into two
Divide spare；
B. by operate a divide a part of ethyl acetate, a part of benzoyl peroxide mixing be put into reaction kettle, at the same time
Butyl acrylate, 2-EHA, hydroxy-ethyl acrylate, dioctyl phthalate and toluene are added, heating is not
It is spare after disconnected stir process 35min；
C. another part ethyl acetate and another part benzoyl peroxide are added into the reaction kettle after operation b processing,
Dilauroyl peroxide, terpene phenol resin, aluminium acetylacetonate, cerium oxide and octadecyl acrylate are added at the same time, and heating is not
Take out spare after disconnected stir process 1h, air is during which constantly passed through into reaction kettle；
D. the mixture for operating gained after c is handled is taken out, after eliminating its interior residual bubbles with ultrasonic wave, is cooled to room
Temperature gets product pressure sensitive adhesive.
Further, step（2）It is 75 DEG C to operate the heating and temperature control described in b, and the speed control of stirring is 350
Rev/min.
Further, step（2）It is 85 DEG C to operate the heating and temperature control described in c, and the speed control of stirring is 500
Rev/min.
Further, step（2）The application frequency for operating the ultrasonic wave described in d is 58kHz.
Embodiment 2
A kind of preparation method of pressure sensitive adhesive for ultrathin double-face glue, includes the following steps：
（1）Raw material weighs spare：
It is spare that following material is weighed by corresponding parts by weight：42 parts of butyl acrylates, 18 parts of 2-EHAs, 3.5
Part hydroxy-ethyl acrylate, 2 parts of dioctyl phthalates, 75 parts of toluene, 58 parts of ethyl acetate, 1.5 parts of benzoyl peroxides, 3
Part dilauroyl peroxide, 30 parts of terpene phenol resins, 1 part of aluminium acetylacetonate, 0.15 part of cerium oxide, 8 parts of octadecyl acrylates；
（2）It is prepared by finished product reaction：
A. first by step（1）The ethyl acetate weighed is divided into two parts, and benzoyl peroxide is equally divided into two
Divide spare；
B. by operate a divide a part of ethyl acetate, a part of benzoyl peroxide mixing be put into reaction kettle, at the same time
Butyl acrylate, 2-EHA, hydroxy-ethyl acrylate, dioctyl phthalate and toluene are added, heating is not
It is spare after disconnected stir process 40min；
C. another part ethyl acetate and another part benzoyl peroxide are added into the reaction kettle after operation b processing,
Dilauroyl peroxide, terpene phenol resin, aluminium acetylacetonate, cerium oxide and octadecyl acrylate are added at the same time, and heating is not
Take out spare after disconnected stir process 1.1h, air is during which constantly passed through into reaction kettle；
D. the mixture for operating gained after c is handled is taken out, after eliminating its interior residual bubbles with ultrasonic wave, is cooled to room
Temperature gets product pressure sensitive adhesive.
Further, step（2）It is 78 DEG C to operate the heating and temperature control described in b, and the speed control of stirring is 380
Rev/min.
Further, step（2）It is 88 DEG C to operate the heating and temperature control described in c, and the speed control of stirring is 520
Rev/min.
Further, step（2）The application frequency for operating the ultrasonic wave described in d is 60kHz.
Embodiment 3
A kind of preparation method of pressure sensitive adhesive for ultrathin double-face glue, includes the following steps：
（1）Raw material weighs spare：
It is spare that following material is weighed by corresponding parts by weight：45 parts of butyl acrylates, 20 parts of 2-EHAs, 4 parts
Hydroxy-ethyl acrylate, 3 parts of dioctyl phthalates, 77 parts of toluene, 60 parts of ethyl acetate, 2 parts of benzoyl peroxides, 3.5 parts
Dilauroyl peroxide, 35 parts of terpene phenol resins, 1.5 parts of aluminium acetylacetonates, 0.2 part of cerium oxide, 10 parts of octadecyl acrylates；
（2）It is prepared by finished product reaction：
A. first by step（1）The ethyl acetate weighed is divided into two parts, and benzoyl peroxide is equally divided into two
Divide spare；
B. by operate a divide a part of ethyl acetate, a part of benzoyl peroxide mixing be put into reaction kettle, at the same time
Butyl acrylate, 2-EHA, hydroxy-ethyl acrylate, dioctyl phthalate and toluene are added, heating is not
It is spare after disconnected stir process 45min；
C. another part ethyl acetate and another part benzoyl peroxide are added into the reaction kettle after operation b processing,
Dilauroyl peroxide, terpene phenol resin, aluminium acetylacetonate, cerium oxide and octadecyl acrylate are added at the same time, and heating is not
Take out spare after disconnected stir process 1.2h, air is during which constantly passed through into reaction kettle；
D. the mixture for operating gained after c is handled is taken out, after eliminating its interior residual bubbles with ultrasonic wave, is cooled to room
Temperature gets product pressure sensitive adhesive.
Further, step（2）It is 80 DEG C to operate the heating and temperature control described in b, and the speed control of stirring is 400
Rev/min.
Further, step（2）It is 90 DEG C to operate the heating and temperature control described in c, and the speed control of stirring is 550
Rev/min.
Further, step（2）The application frequency for operating the ultrasonic wave described in d is 62kHz.
Comparative example 1
This comparative example 1 compared with Example 2, in step（2）Saved in finished product reaction preparation manipulation c in whereabouts reaction kettle
The processing of air is passed through, method and step all same in addition.
Comparative example 2
This comparative example 2 compared with Example 2, in step（1）Raw material weighs spare and step（2）It is prepared by finished product reaction
In eliminate cerium oxide component, method and step all same in addition.
Comparative example 3
This comparative example 3 compared with Example 2, in step（1）Raw material weighs spare and step（2）It is prepared by finished product reaction
In eliminate cerium oxide and octadecyl acrylate component, method and step all same in addition.
Control group
A kind of pressure sensitive adhesive prepared by Application No. 201410371874.8.
In order to contrast effect of the present invention, to above-described embodiment 2, comparative example 1, comparative example 2, comparative example 3,
Pressure sensitive adhesive obtained by control group is tested for the property, and double faced adhesive tape is made according to Same Way, concrete operations are：Pressure sensitive adhesive is used
The surface that bar is spread evenly across 4 μm of PET base materials forms straight rubberised layer, and pressure sensitive adhesive is applied in release liners or release film
It is posted to be formed on another surface of PET base materials again and is posted glue-line, then by equipped with straight rubberised layer and the PET base materials for being posted glue-line
It is made respectively through 100 DEG C of baking 2min；Straight rubberised layer and be posted glue-line it is toasted after formed respectively and straight apply drying adhesive layer and be posted dry
Glue-line, the straight thickness for applying drying adhesive layer and being posted drying adhesive layer is 5 μm；Finally double faced adhesive tape made from each group is tested for the property,
Specific correction data see the table below shown in 1：
Table 1
Note：Retentivity A described in upper table 1：Test under 1xlin areas and the holding of 1kg counterweights is hung in 70 DEG C/83 DEG C
Power；Retentivity B：Test under 1xlin areas in the retentivity of room temperature hanging 2kg counterweights.
Preparation method of the present invention can be obviously improved the use caking property of pressure sensitive adhesive at high temperature it can be seen from upper table 1
Can, it is stronger using quality higher, competitiveness.
Claims (4)
1. the preparation method of a kind of pressure sensitive adhesive for ultrathin double-face glue, it is characterised in that include the following steps：
（1）Raw material weighs spare：
It is spare that following material is weighed by corresponding parts by weight：40 ~ 45 parts of butyl acrylates, 15 ~ 20 parts of 2-EHAs, 3 ~
4 parts of hydroxy-ethyl acrylates, 1 ~ 3 part of dioctyl phthalate, 73 ~ 77 parts of toluene, 55 ~ 60 parts of ethyl acetate, 1 ~ 2 part of peroxidating
Benzoyl, 2.5 ~ 3.5 parts of dilauroyl peroxides, 25 ~ 35 parts of terpene phenol resins, 0.5 ~ 1.5 part of aluminium acetylacetonate, 0.1 ~ 0.2
Part cerium oxide, 5 ~ 10 parts of octadecyl acrylates；
（2）It is prepared by finished product reaction：
A. first by step（1）The ethyl acetate weighed is divided into two parts, and it is standby that benzoyl peroxide is equally divided into two parts
With；
B. by operate a divide a part of ethyl acetate, a part of benzoyl peroxide mixing be put into reaction kettle, add at the same time
Butyl acrylate, 2-EHA, hydroxy-ethyl acrylate, dioctyl phthalate and toluene, heat and constantly stir
Mix spare after 35 ~ 45min of processing；
C. another part ethyl acetate and another part benzoyl peroxide are added into the reaction kettle after operation b processing, at the same time
Dilauroyl peroxide, terpene phenol resin, aluminium acetylacetonate, cerium oxide and octadecyl acrylate are added, heats and constantly stirs
Mix and take out after 1 ~ 1.2h of processing spare, air is during which constantly passed through into reaction kettle；
D. the mixture for operating gained after c is handled is taken out, after eliminating its interior residual bubbles with ultrasonic wave, is cooled to room temperature i.e.
Obtain finished product pressure sensitive adhesive.
A kind of 2. preparation method of pressure sensitive adhesive for ultrathin double-face glue according to claim 1, it is characterised in that step
（2）It is 75 ~ 80 DEG C to operate the heating and temperature control described in b, and the speed control of stirring is 350 ~ 400 revs/min.
A kind of 3. preparation method of pressure sensitive adhesive for ultrathin double-face glue according to claim 1, it is characterised in that step
（2）It is 85 ~ 90 DEG C to operate the heating and temperature control described in c, and the speed control of stirring is 500 ~ 550 revs/min.
A kind of 4. preparation method of pressure sensitive adhesive for ultrathin double-face glue according to claim 1, it is characterised in that step
（2）The application frequency for operating the ultrasonic wave described in d is 58 ~ 62kHz.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710501176.9A CN107216432B (en) | 2017-06-27 | 2017-06-27 | A kind of preparation method of pressure sensitive adhesive for ultrathin double-face glue |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710501176.9A CN107216432B (en) | 2017-06-27 | 2017-06-27 | A kind of preparation method of pressure sensitive adhesive for ultrathin double-face glue |
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|---|---|
| CN107216432A CN107216432A (en) | 2017-09-29 |
| CN107216432B true CN107216432B (en) | 2018-04-13 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602919A (en) * | 2009-06-18 | 2009-12-16 | 永大（中山）有限公司 | Double-sided pressure-sensitive adhesive tape that computer embroidery is used and preparation method thereof |
| CN101978014A (en) * | 2008-03-17 | 2011-02-16 | 日东电工株式会社 | Acrylic pressure-sensitive adhesive, acrylic pressure-sensitive adhesive layer and acrylic pressure-sensitive adhesive tape or sheet |
| CN104087215A (en) * | 2014-07-31 | 2014-10-08 | 东莞宏石功能材料科技有限公司 | Pressure-sensitive adhesive applied to ultra-thin double faced adhesive tape and preparation method of pressure-sensitive adhesive |
| CN104277653A (en) * | 2014-09-29 | 2015-01-14 | 潜伟清 | Ultrathin high-temperature-resistant thermal-insulation paint |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07331209A (en) * | 1994-06-15 | 1995-12-19 | Sekisui Chem Co Ltd | Acrylic tack agent composition |
-
2017
- 2017-06-27 CN CN201710501176.9A patent/CN107216432B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101978014A (en) * | 2008-03-17 | 2011-02-16 | 日东电工株式会社 | Acrylic pressure-sensitive adhesive, acrylic pressure-sensitive adhesive layer and acrylic pressure-sensitive adhesive tape or sheet |
| CN101602919A (en) * | 2009-06-18 | 2009-12-16 | 永大（中山）有限公司 | Double-sided pressure-sensitive adhesive tape that computer embroidery is used and preparation method thereof |
| CN104087215A (en) * | 2014-07-31 | 2014-10-08 | 东莞宏石功能材料科技有限公司 | Pressure-sensitive adhesive applied to ultra-thin double faced adhesive tape and preparation method of pressure-sensitive adhesive |
| CN104277653A (en) * | 2014-09-29 | 2015-01-14 | 潜伟清 | Ultrathin high-temperature-resistant thermal-insulation paint |
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Effective date of registration: 20180530 Address after: 518116 Shenzhen, Longgang, Guangdong Longgang District, Longgang street, Wulian community, 165-2, 1-2. Patentee after: Shenzhen Guoxing Xiang adhesive materials Co., Ltd. Address before: 236300 Funan County Industrial Park in Fuyang, Anhui Patentee before: Funan County Wei Wei packing material Co., Ltd. |