CN104562704A - Pre-treatment method of long glass fiber yarn - Google Patents
Pre-treatment method of long glass fiber yarn Download PDFInfo
- Publication number
- CN104562704A CN104562704A CN201410848316.6A CN201410848316A CN104562704A CN 104562704 A CN104562704 A CN 104562704A CN 201410848316 A CN201410848316 A CN 201410848316A CN 104562704 A CN104562704 A CN 104562704A
- Authority
- CN
- China
- Prior art keywords
- glass fiber
- fiber yarn
- minutes
- yarn
- pa10t
- 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
- 239000003365 glass fiber Substances 0.000 title claims abstract description 54
- 238000002203 pretreatment Methods 0.000 title abstract 5
- 238000000034 method Methods 0.000 claims abstract description 35
- 229920006119 nylon 10T Polymers 0.000 claims abstract description 32
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- 238000005507 spraying Methods 0.000 claims abstract description 3
- 239000007921 spray Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000005096 rolling process Methods 0.000 claims description 9
- 229920006111 poly(hexamethylene terephthalamide) Polymers 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229920006115 poly(dodecamethylene terephthalamide) Polymers 0.000 claims description 5
- 229920006128 poly(nonamethylene terephthalamide) Polymers 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 238000002791 soaking Methods 0.000 abstract description 2
- 238000005470 impregnation Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 239000011521 glass Substances 0.000 description 12
- 239000000243 solution Substances 0.000 description 8
- 230000014759 maintenance of location Effects 0.000 description 7
- 239000004677 Nylon Substances 0.000 description 3
- 239000011152 fibreglass Substances 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 239000004696 Poly ether ether ketone Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- -1 aliphatic diamine Chemical class 0.000 description 1
- 229920003233 aromatic nylon Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920006012 semi-aromatic polyamide Polymers 0.000 description 1
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Surface Treatment Of Glass Fibres Or Filaments (AREA)
Abstract
The invention provides a pre-treatment method of a long glass fiber yarn. The pre-treatment method comprises the following steps: step 1, carrying out heat preservation for 5-10 minutes on the glass fiber yarn at a temperature of 150-200 DEG C; step 2, soaking for 5-10 minutes in a concentrated sulfuric acid solution containing PA10T; step 3, atomizing with deionized water and staying for 5-10 minutes; step 4, spraying with deionized water till the PH on the surface is higher than or equal to 6.5 and removing redundant sulfuric acid; step 5, drying for 30-60 minutes at a temperature of 100 DEG C. The pre-treatment method solves the problem that a long glass fiber reinforced PA10T material with high glass fiber content cannot be prepared according to the conventional melt impregnation process. The invention belongs to the field of pre-treatment of glass fiber yarns.
Description
Technical field
The present invention relates to a kind of preprocess method, be specifically related to a kind of preprocess method making the surface grafting PA10T of glass fiber yarn.
Background technology
Nylon 10T(PA10T) be high temperature resistant semi-aromatic nylon, be obtaining through polycondensation, is the one of aromatic nylon by the diacid of aliphatic diamine or diacid and band aromatic rings or diamines.Owing to having imported aromatic rings in nylon molecules main chain section, thus improve heat resistance and mechanical property, reduce water absorption rate etc., and there is good cost performance, be the resin that heat resistance between general engineering plastic nylon and thermostability engineering plastic PEEK is high, be mainly used in automobile and electric and electronic industry.Because the processing temperature Sum decomposition temperature of PA10T is close, so PA10T material is while processing, material can decompose to some extent.The long glass fiber reinforced PA10T material of high-load glass (being greater than 60%) cannot be prepared particularly by melt impregnating process, mainly in impregnating equipment, glass fiber yarn is difficult to dispersion, PA10T material cannot be filled in interface, cause the long glass fiber reinforced PA10T material product surface difference of injection moulding, glass (glass fibre) is reunited serious.
Summary of the invention
The object of the invention is to: the long glass fiber reinforced PA10T material cannot preparing high-load glass for existing melt impregnating process, provides a kind of preprocess method of long glass fibres yarn.
The solution of the present invention is as follows: a kind of preprocess method of long glass fibres yarn, comprises following processing step: the first step: glass fiber yarn is incubated 5 ~ 10 minutes under 150 ~ 200 DEG C of temperature conditions; Second step: glass fiber yarn is soaked 5 ~ 10 minutes in containing the concentrated sulfuric acid solution of PA10T; 3rd step: glass fiber yarn is sprayed with deionized water, 5 ~ 10 minutes time of staying; 4th step: spray glass fiber yarn with deionized water, until surperficial PH >=6.5; 5th step: glass fiber yarn is dried.
Preferably, the glass fiber yarn after process is wound around rolling.
Preferably, after the described first step completes, glass fiber yarn is taken out and is cooled to normal temperature, then carry out lower continuous step again.
Preferably, under first step heating condition, glass fiber yarn is fixed by depression bar and is formed the arrangement that cross section is w type, in the arrangement of described W type, angle b >=90 ° on the middle both sides of composition W, described both sides and both sides end points line form in triangle, a >=60 °, angle of one of another two jiaos except the b of angle, and the distribution of fiberglass fiber yarn is greater than and equals 1.5 these W type structures.
Preferably, in described concentrated sulfuric acid solution, the concentration of PA10T is 0.02 ~ 0.1g/ml, after ensureing process, and content >=0.5% (mass fraction) of the PA10T of fiberglass surfacing grafting and coating.
Preferably, the described concentrated sulfuric acid solution containing PA10T can be replaced with the concentrated sulfuric acid solution containing PA6T, PA9T or PA12T, thus prepare the glass fiber yarn of surface grafting PA6T, PA9T or PA12T.
Preferably, gases used during spraying is nitrogen, utilizes nitrogen to protect PA10T, prevents PA10T to be oxidized.
Beneficial effect of the present invention: fiberglass fiber yarn is sprayed with deionized water after soaking again, and the concentration of the concentrated sulfuric acid is reduced, PA10T separates out on glass surface, and utilize concentrated sulfuric acid water suction to produce a large amount of heats to promote that glass surface produces graft reaction, unnecessary sulfuric acid is removed again through spray, thus prepare the glass fiber yarn of surface grafting PA10T, simultaneously, concentrated sulfuric acid solution containing PA10T is replaced with containing PA6T, the concentrated sulfuric acid solution of PA9T or PA12T, thus surface grafting PA6T can be prepared, the glass fiber yarn of PA9T or PA12T, it is simple that glass fiber yarn after the method for the invention process has process, formation efficiency is high, cost is low, the advantages such as steady quality, be suitable for the large-scale production preparing high-load long glass fiber reinforced high-temperature nylon master batch.
Accompanying drawing explanation
Fig. 1 is the sectional view (being arranged into 2 described W type structures of glass fiber yarn) of glass fiber yarn of the present invention arrangement.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearly, the present invention is described in further detail below with reference to accompanying drawings,
Embodiment 1:
Trade mark ER4301 alkali-free glass fibre yarn (2400 tex) is put into the baking oven of 160 ± 10 DEG C of heating up, glass is arranged by structure shown in Fig. 1 in an oven, temperature retention time 10 minutes, taking-up is cooled to normal temperature, then being immersed 50L contains in the concentrated sulfuric acid of PA10T, and PA10T is 0.04g/ml in concentrated sulfuric acid concentration, soaks after 10 minutes and takes out, then process deionized water is sprayed, 10 minutes time of staying.Process deionized water sprays again, until surperficial PH is greater than 6.5, finally put into drying baker 100 DEG C of taking-ups in 60 minutes and namely obtain product through being wound around rolling, after tested, in obtained product, the content of PA10T is 1.53%(mass fraction).
Embodiment 2:
Trade mark ER4301 alkali-free glass fibre yarn (2400 tex) is put into the baking oven of 170 ± 10 DEG C of heating up, glass is arranged by structure shown in Fig. 1 in an oven, temperature retention time 8 minutes, taking-up is cooled to normal temperature, then immersed 50L, PA10T is 0.04g/ml in concentrated sulfuric acid concentration, soaks after 8 minutes and takes out, then process deionized water is sprayed, 8 minutes time of staying.Process deionized water sprays again, until surperficial PH is greater than 6.5, finally put into drying baker 100 DEG C of taking-ups in 50 minutes and namely obtain product through being wound around rolling, after tested, in obtained product, the content of PA10T is 1.13%(mass fraction).
Embodiment 3:
Trade mark ER4301 alkali-free glass fibre yarn (2400 tex) is put into the baking oven of 180 ± 10 DEG C of heating up, glass is arranged by structure shown in Fig. 1 in an oven, temperature retention time 7 minutes, taking-up is cooled to normal temperature, then immersed 50L, PA10T is 0.04g/ml in concentrated sulfuric acid concentration, soaks after 7 minutes and takes out, then process deionized water is sprayed, 7 minutes time of staying.Process deionized water sprays again, until surperficial PH is greater than 6.5, finally put into drying baker 100 DEG C of taking-ups in 40 minutes and namely obtain product through being wound around rolling, after tested, in obtained product, the content of PA10T is 0.73%(mass fraction).
Embodiment 4:
Trade mark ER4301 alkali-free glass fibre yarn (2400 tex) is put into the baking oven of 190 ± 10 DEG C of heating up, glass is arranged by structure shown in Fig. 1 in an oven, temperature retention time 6 minutes, taking-up is cooled to normal temperature, is then immersed 50L, and PA10T is 0.04g/ml in concentrated sulfuric acid concentration, soak after 10 minutes and take out, then process deionized water is sprayed, 6 minutes time of staying.Process deionized water sprays again, until surperficial PH is greater than 6.5, finally put into drying baker 100 DEG C of taking-ups in 30 minutes and namely obtain product through being wound around rolling, after tested, in obtained product, the content of PA10T is 0.52%(mass fraction).
Embodiment 5:
Trade mark ER4301 alkali-free glass fibre yarn (2400 tex) is put into the baking oven of 160 ± 10 DEG C of heating up, glass is arranged by structure shown in Fig. 1 in an oven, temperature retention time 10 minutes, taking-up is cooled to normal temperature, then immersed 50L, PA6T is 0.04g/ml in concentrated sulfuric acid concentration, soaks after 10 minutes and takes out, then process deionized water is sprayed, 10 minutes time of staying.Process deionized water sprays again, until surperficial PH is greater than 6.5, finally puts into drying baker 100 DEG C of taking-ups in 60 minutes and namely obtains product through being wound around rolling.
Embodiment 6:
Trade mark ER4301 alkali-free glass fibre yarn (2400 tex) is put into the baking oven of 160 ± 10 DEG C of heating up, glass is arranged by structure shown in Fig. 1 in an oven, temperature retention time 10 minutes, taking-up is cooled to normal temperature, is then immersed 50L, and PA6T is 0.08g/ml in concentrated sulfuric acid concentration, soak after 10 minutes and take out, then process deionized water is sprayed, 10 minutes time of staying.Process deionized water sprays again, until surperficial PH is greater than 6.5, finally puts into drying baker 100 DEG C of taking-ups in 60 minutes and namely obtains product through being wound around rolling.
Embodiment 7:
Trade mark ER4301 alkali-free glass fibre yarn (2400 tex) is put into the baking oven of 160 ± 10 DEG C of heating up, glass is arranged by structure shown in Fig. 1 in an oven, temperature retention time 10 minutes, taking-up is cooled to normal temperature, is then immersed 50L, and PA6T is 0.10g/ml in concentrated sulfuric acid concentration, soak after 10 minutes and take out, then process deionized water is sprayed, 10 minutes time of staying.Process deionized water sprays again, until surperficial PH is greater than 6.5, finally puts into drying baker 100 DEG C of taking-ups in 60 minutes and namely obtains product through being wound around rolling.
Claims (8)
1. a preprocess method for long glass fibres yarn, is characterized in that comprising following processing step: the first step: glass fiber yarn (1) is incubated 5 ~ 10 minutes under 150 ~ 200 DEG C of temperature conditions; Second step: glass fiber yarn (1) is soaked 5 ~ 10 minutes in containing the concentrated sulfuric acid solution of PA10T; 3rd step: glass fiber yarn (1) is sprayed with deionized water, 5 ~ 10 minutes time of staying; 4th step: spray glass fiber yarn (1) with deionized water, until surperficial PH >=6.5; 5th step: glass fiber yarn (1) is dried.
2. the preprocess method of a kind of long glass fibres yarn according to claim 1, is characterized in that: after the described first step completes, and is taken out by glass fiber yarn (1) and is cooled to normal temperature, then carry out lower continuous step again.
3. the preprocess method of a kind of long glass fibres yarn according to claim 1, is characterized in that: under first step heating condition, and glass fiber yarn (1) forms by depression bar (2) is fixing the arrangement that cross section is w type.
4. the preprocess method of a kind of long glass fibres yarn according to claim 2, it is characterized in that: in the arrangement of described W type, angle b >=90 ° on the middle both sides of composition W, described both sides and both sides end points line form in triangle, a >=60 °, angle of one of another two jiaos except the b of angle, and the arrangement of glass fiber yarn 1 is greater than and equals 1.5 these W type structures.
5. the preprocess method of a kind of long glass fibres yarn according to claim 1, is characterized in that: the technological parameter of baking step is 100 DEG C, 30 ~ 60 minutes, after oven dry, and glass fiber yarn (1) is wound around rolling.
6. the preprocess method of a kind of long glass fibres yarn according to claim 1, is characterized in that: in described concentrated sulfuric acid solution, the concentration of PA10T is 0.02 ~ 0.1g/ml.
7. a kind of preprocess method of long glass fibres yarn according to claim 1 or 6, is characterized in that: the described concentrated sulfuric acid solution containing PA10T is replaced with the concentrated sulfuric acid solution containing PA6T, PA9T or PA12T.
8. the preprocess method of a kind of long glass fibres yarn according to claim 1, is characterized in that: gases used during spraying is nitrogen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410848316.6A CN104562704B (en) | 2014-12-31 | 2014-12-31 | A kind of preprocess method of long glass fibres yarn |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410848316.6A CN104562704B (en) | 2014-12-31 | 2014-12-31 | A kind of preprocess method of long glass fibres yarn |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104562704A true CN104562704A (en) | 2015-04-29 |
| CN104562704B CN104562704B (en) | 2016-08-17 |
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| CN201410848316.6A Active CN104562704B (en) | 2014-12-31 | 2014-12-31 | A kind of preprocess method of long glass fibres yarn |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101405329A (en) * | 2006-03-13 | 2009-04-08 | 旭化成化学株式会社 | Process for production of glass fiber-reinforced polyamide resin composition |
| CN103013098A (en) * | 2012-11-26 | 2013-04-03 | 江苏金发科技新材料有限公司 | Halogen-free flame-retardant continuous long glass fiber reinforced polyamide 6 composite material and preparation method thereof |
| CN103072292A (en) * | 2013-01-09 | 2013-05-01 | 金发科技股份有限公司 | Molding device and preparation method for long fiber-reinforced nylon |
| CN103450491A (en) * | 2013-09-23 | 2013-12-18 | 上海纳岩新材料科技有限公司 | Long-glass-fiber reinforced nylon 6 composite material and preparation method thereof |
| US20140364025A1 (en) * | 2013-06-11 | 2014-12-11 | Johns Manville | Fiber-reinforced composite articles and methods of making them |
| CN104210113A (en) * | 2014-07-09 | 2014-12-17 | 贵州凯科特材料有限公司 | High-performance long glass fiber reinforced nylon 10T composite material and preparation method thereof |
-
2014
- 2014-12-31 CN CN201410848316.6A patent/CN104562704B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101405329A (en) * | 2006-03-13 | 2009-04-08 | 旭化成化学株式会社 | Process for production of glass fiber-reinforced polyamide resin composition |
| CN103013098A (en) * | 2012-11-26 | 2013-04-03 | 江苏金发科技新材料有限公司 | Halogen-free flame-retardant continuous long glass fiber reinforced polyamide 6 composite material and preparation method thereof |
| CN103072292A (en) * | 2013-01-09 | 2013-05-01 | 金发科技股份有限公司 | Molding device and preparation method for long fiber-reinforced nylon |
| US20140364025A1 (en) * | 2013-06-11 | 2014-12-11 | Johns Manville | Fiber-reinforced composite articles and methods of making them |
| CN103450491A (en) * | 2013-09-23 | 2013-12-18 | 上海纳岩新材料科技有限公司 | Long-glass-fiber reinforced nylon 6 composite material and preparation method thereof |
| CN104210113A (en) * | 2014-07-09 | 2014-12-17 | 贵州凯科特材料有限公司 | High-performance long glass fiber reinforced nylon 10T composite material and preparation method thereof |
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| Publication number | Publication date |
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| CN104562704B (en) | 2016-08-17 |
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Denomination of invention: Pre-treatment method of long glass fiber yarn Effective date of registration: 20180504 Granted publication date: 20160817 Pledgee: Baiyun branch of Guiyang Bank Co., Ltd. Pledgor: Guizhou Kaikete Material Co., Ltd. Registration number: 2018520000006 |
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Denomination of invention: Pre-treatment method of long glass fiber yarn Effective date of registration: 20180607 Granted publication date: 20160817 Pledgee: Baiyun branch of Guiyang Bank Co., Ltd. Pledgor: Guizhou Kaikete Material Co., Ltd. Registration number: 2018520000007 |
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Denomination of invention: Pre-treatment method of long glass fiber yarn Effective date of registration: 20190926 Granted publication date: 20160817 Pledgee: Baiyun branch of Guiyang Bank Co., Ltd. Pledgor: Guizhou Kaikete Material Co., Ltd. Registration number: Y2019520000009 |
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