CN105884214A - Preparation method of conductive glass fibers - Google Patents
Preparation method of conductive glass fibers Download PDFInfo
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- CN105884214A CN105884214A CN201610211331.9A CN201610211331A CN105884214A CN 105884214 A CN105884214 A CN 105884214A CN 201610211331 A CN201610211331 A CN 201610211331A CN 105884214 A CN105884214 A CN 105884214A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/24—Coatings containing organic materials
- C03C25/26—Macromolecular compounds or prepolymers
- C03C25/28—Macromolecular compounds or prepolymers obtained by reactions involving only carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/42—Coatings containing inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/66—Chemical treatment, e.g. leaching, acid or alkali treatment
- C03C25/68—Chemical treatment, e.g. leaching, acid or alkali treatment by etching
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- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention provides a preparation method of conductive glass fibers. The method comprises the steps that alkali-free glass fibers are immersed in an aqueous hydrochloric acid solution, after immersing is completed, the immersed glass fibers are fully rinsed with water and dried, and hydroxylated glass fibers are obtained; the hydroxylated glass fibers are immersed in an aqueous polyethyleneimine solution, after immersing is completed, the immersed glass fibers are fully rinsed with water and dried, and glass fibers surface-modified with polyethyleneimine are obtained; the glass fibers surface-modified with polyethyleneimine are put into an aqueous copper sulfate pentahydrate solution, after immersing is conducted, an aqueous sodium thiosulfate solution is added, the immersed glass fibers are taken out after a reaction is conducted, rinsed with water and dried, and cuprous sulfide and glass fiber composite conductive fibers are obtained. The technology is adopted for preparing the conductive glass fibers, equipment used in the technology is low in investment cost, operation is easy, the reaction condition is mild, the applicability is high, the treatment effect is good, the fiber performance loss is low, the quality is reliable, environmental pollution can be reduced, and the method is suitable for industrial production.
Description
Technical field
The present invention relates to conductive fiber preparation field, particularly relate to the preparation method of a kind of electroconductive glass fibre.
Background technology
In recent years, along with developing rapidly and universal of computer, telecommunications, microwave oven etc., human lives works
Electromagnetic radiation in environment is day by day serious, thus the normal work that the Electromagnetic Interference produced is to electronic equipment
Make and the physiological health of the mankind brings a lot of negative effect.For preventing static interference and Electromagnetic Interference, from
Mid-term in 20th century so far, has developed the material of various antistatic and electromagnetic shielding.Recent decades, research
Emphasis has turned to conductive fiber more, and the antistatic effect of conductive fiber is more significantly persistently, and not by ring
The impact of border humidity, conductive layer reaches certain thickness or after conductive component reaches certain proportion, has excellent electromagnetism
Function of shielding, therefore development and the application of conductive fiber increasingly comes into one's own.
Glass fibre is a kind of new function material in Inorganic Non-metallic Materials and structural material.Owing to it has
Have noninflammability, high temperature resistant, anticorrosive, intensity is high, density is little, moisture absorption is low and extends a series of excellences such as little
Characteristic, be widely used to traditional industry, agricultural, building industry and electronics, communication, nuclear energy, aviation,
Space flight, weapons, naval vessels and the high and new technology industry such as ocean development, genetic engineering, become the 21 century mankind not
The new and high technology material of the sustainable development that can lack.In recent years, many researcheres attempt by modern chemistry,
The method modified glass-fibers such as physics, prepare the electroconductive glass fibre conductive filler as polymer composite
Material, be used for solving Contamination of Electromagnetic Wave problem.Chemical plating is as material surface metalized technology,
Through becoming one of conventional technology of electroconductive glass fibre of preparing, but traditional glass fibre chemistry plating Yin Qishi
Need during plating matrix is slightly spent, sensitization, activation processing, not only complex process, and activated
The heavy metal palladium needed in journey is expensive, and these all limit electroless plating method and prepare entering of electroconductive glass fibre
One step development.Therefore, develop new, effectively to prepare electroconductive glass fibre method to have great importance.
Metal sulfide all has special performance at aspects such as optics, Optical Electro-Chemistry, catalysis, environmental protection.It
There is good chemically and thermally stability, be a kind of good photoelectric material.Utilize the spy of metal sulfide
Property produce the method for conductive fiber application at present most be fiber surface chemical reaction method, this method
Main by chemical treatment, i.e. by the dipping of reactant liquor, produce absorption at fiber surface, then by changing
Learning reaction makes metal sulfide cover at fiber surface.The method advantage is that technique is simple, cost is relatively low,
And it is less to the intensity of fiber, flexibility, slipping equivalent damage.In the eighties in 20th century, Japan is just
It is developed into this kind of conductive fiber.Conductive compositions and electrical conduction mechanism are also studied, such as Japan by specially
The surface developed covers the conductive acrylic fibre of the sulfide of copper, is first to be processed in copper ions solution by acrylon,
Then process in reducing agent, the Cu on fiber2+Become Cu+With-CN complexation, form the sulfuration of copper further
The conductive material of thing.Owing to these conductive materials define network on fibre structure, therefore electric conductivity is very
Good.Domestic patents 87104625.3,201510188325.1,200810084225.4 etc. are all to use this side
Method produces conductive fiber.Owing to the cyano group on polyacrylonitrile fibre can produce complexation with copper ion, make fiber
There is electric conductivity;Common fiberglass surfacing lacks the group with copper ion complexation, and conductive materials just cannot
With fiber generation complexation, therefore have impact on absorption and the absorption fastness of fiber thing thio to metal, therefore cannot make
Obtain the conductive fiber that electric conductivity is excellent.
Summary of the invention
It is an object of the invention to, it is provided that the preparation method of a kind of electroconductive glass fibre, solve prior art
The absorption fastness of middle fiber thing thio to metal is low, it is impossible to the problem preparing the excellent conductive fiber of electric conductivity.
The present invention by the following technical solutions, proposes the preparation method of a kind of electroconductive glass fibre, the steps include:
(1) alkali-free glass fibre is immersed in aqueous hydrochloric acid solution in 20 DEG C~50 DEG C immersions 0.5~2 hour,
After immersion, fully rinse with water, obtain hydroxylating glass fibre after drying;
(2) hydroxylating glass fibre step (1) obtained immerses the polyethyleneimine that concentration is 0.5%~2%
In amine aqueous solution, soak 2~6 hours at 60 DEG C~90 DEG C, after immersion, fully rinse with water, be dried
After obtain polymine surface modify glass fibre;
(3) glass fibre that polymine surface step (2) obtained is modified is placed in mass concentration and is
In 2.5%~10% copper sulphate pentahydrate aqueous solution, after soaking 5~30 minutes at 20 DEG C~60 DEG C, add quality dense
Degree is 2.5%~5% sodium thiosulfate solution, is warming up to 75 DEG C~90 DEG C and reacts 0.3~1.5 hour, after taking-up
Cuprous sulfide/glass fibre composite conducting fiber is obtained after water rinsing, drying.
In described step (1), aqueous hydrochloric acid solution concentration is 1mol/L~3mol/.
In described step (3) mass ratio of copper sulphate pentahydrate aqueous solution and sodium thiosulfate solution be 1:1~
1:2.
The invention has the beneficial effects as follows:
(1) glass fibre is carried out immersion treatment initially with dilute hydrochloric acid by the present invention, then in fiber surface shape
Become polyethyleneimine amine layer, use chemical reaction method to generate cuprous sulfide at fiber surface on this basis and answered
Close electroconductive glass fibre.The immersion of dilute hydrochloric acid not only makes fiberglass surfacing crack and hollow, and will
Fiber surface introduces carbonyl;Polymine is stronger hydrogen-bond donor, and forms strong hydrogen bond between carbonyl
Interacting, this strong interaction makes polymine be firmly adhered to fiberglass surfacing;Separately
Outward, polymine is a kind of typical cationic water-soluble polymer electrolyte, macromolecular chain has big
The amido atom N of amount makes it have the strongest electron acceptor, and it can produce the strongest complexing to copper ion,
The absorption on the fiber surface of the sulfide of raising copper.In the present invention metal sulfide and glass fiber matrix it
Between by the strongest adhesion of " bridge formation " of polyethyleneimine amine layer effect formation, improve cuprous sulfide in glass fibers
Content in dimension, really solves the glass fibre active adsorption problem to metal sulfide, and fiber has surely
Fixed, lasting conductive effect.
(2) using the technique of the present invention to prepare electroconductive glass fibre, device therefor investment cost is low, operation letter
List, reaction condition are gentle, the suitability is strong, the loss of high treating effect, fibre property is few, reliable in quality, and
And environmental pollution can be reduced, it is adaptable to industrialized production.
Detailed description of the invention
Embodiment 1
The present invention proposes the preparation method of a kind of electroconductive glass fibre, the steps include:
(1) alkali-free glass fibre that 10 grams clean up being immersed in 200 grams of concentration is the hydrochloric acid water of 1mol/L
In solution, soak 0.5 hour in 50 DEG C, after immersion, fully rinse with water, obtain hydroxylating after drying
Glass fibre;
(2) hydroxylating glass fibre prepared by step (1) is immersed the poly-second that 200 gram mass concentration are 0.5%
In alkene imines aqueous solution, soak 4 hours at 60 DEG C, after immersion, fully rinse with water, obtain after drying
The glass fibre that polymine surface is modified;
(3) it is dense that the glass fibre that polymine surface step (2) prepared is modified is placed in 150 gram masses
Degree is in the copper sulphate pentahydrate aqueous solution of 2.5%, and after soaking 5 minutes at 60 DEG C, adding 150 gram mass concentration is
2.5% sodium thiosulfate solution, is warming up to 75 DEG C and reacts 1.5 hours, rinses with water, dries after taking out fiber
After obtain cuprous sulfide/glass fibre composite conducting fiber, the electrical conductivity of fiber is 2.0 × 10-2S/cm。
Embodiment 2
The present invention proposes the preparation method of a kind of electroconductive glass fibre, the steps include:
(1) alkali-free glass fibre that 10 grams clean up being immersed in 150 grams of concentration is the hydrochloric acid water of 2mol/L
In solution, soak 2 hours in 20 DEG C, after immersion, fully rinse with water, obtain hydroxylating glass after drying
Glass fiber;
(2) hydroxylating glass fibre prepared by step (1) is immersed the poly-second that 200 gram mass concentration are 0.5%
In alkene imines aqueous solution, soak 6 hours at 90 DEG C, after immersion, fully rinse with water, obtain after drying
The glass fibre that polymine surface is modified;
(3) it is dense that the glass fibre that polymine surface step (2) prepared is modified is placed in 150 gram masses
Degree is in the copper sulphate pentahydrate aqueous solution of 5%, and after soaking 5 minutes at 60 DEG C, adding 150 gram mass concentration is 5%
Sodium thiosulfate solution, is warming up to 90 DEG C and reacts 0.3 hour, obtains after taking out fiber after water rinsing, drying
To cuprous sulfide/glass fibre composite conducting fiber, the electrical conductivity of fiber is 6.2 × 10-2S/cm。
Embodiment 3
The present invention proposes the preparation method of a kind of electroconductive glass fibre, the steps include:
(1) alkali-free glass fibre that 10 grams clean up being immersed in 150 grams of concentration is the hydrochloric acid water of 3mol/L
In solution, soak 1 hour in 30 DEG C, after immersion, fully rinse with water, obtain hydroxylating glass after drying
Glass fiber;
(2) hydroxylating glass fibre prepared by step (1) is immersed the poly-second that 200 gram mass concentration are 1.5%
In alkene imines aqueous solution, soak 5 hours at 80 DEG C, after immersion, fully rinse with water, obtain after drying
The glass fibre that polymine surface is modified;
(3) it is dense that the glass fibre that polymine surface step (2) prepared is modified is placed in 150 gram masses
Degree is in the copper sulphate pentahydrate aqueous solution of 10%, and after soaking 30 minutes at 20 DEG C, adding 300 gram mass concentration is
5% sodium thiosulfate solution, is warming up to 80 DEG C and reacts 1.0 hours, after rinsing with water, dry after taking out fiber
Obtaining cuprous sulfide/glass fibre composite conducting fiber, the electrical conductivity of fiber is 1.3 × 100S/cm。
Embodiment 4
The present invention proposes the preparation method of a kind of electroconductive glass fibre, the steps include:
(1) alkali-free glass fibre that 10 grams clean up being immersed in 150 grams of concentration is the hydrochloric acid water of 1.5mol/L
In solution, soak 1.5 hours in 30 DEG C, after immersion, fully rinse with water, obtain hydroxylating after drying
Glass fibre;
(2) hydroxylating glass fibre prepared by step (1) is immersed the poly-second that 200 gram mass concentration are 1.0%
In alkene imines aqueous solution, soak 2 hours at 90 DEG C, after immersion, fully rinse with water, obtain after drying
The glass fibre that polymine surface is modified;
(3) glass fibre that polymine surface step (2) prepared is modified is placed in 150 grams of concentration and is
In the copper sulphate pentahydrate aqueous solution of 8%, after soaking 20 minutes at 30 DEG C, adding 280 gram mass concentration is 4.5%
Sodium thiosulfate solution, is warming up to 75 DEG C and reacts 1.0 hours, obtains after taking out fiber after water rinsing, drying
To cuprous sulfide/glass fibre composite conducting fiber, the electrical conductivity of fiber is 4.8 × 10-1S/cm。
Embodiment 5
The present invention proposes the preparation method of a kind of electroconductive glass fibre, the steps include:
(1) alkali-free glass fibre that 10 grams clean up being immersed in 150 grams of concentration is the hydrochloric acid water of 2.5mol/L
In solution, soak 2 hours in 30 DEG C, after immersion, fully rinse with water, obtain hydroxyl by after fiber drying
The glass fibre of base;
(2) hydroxylating glass fibre prepared by step (1) is immersed the poly-second that 200 gram mass concentration are 2.5%
In alkene imines aqueous solution, soak 5 hours at 70 DEG C, after immersion, fully rinse with water, obtain after drying
The glass fibre that polymine surface is modified;
(3) it is dense that the glass fibre that polymine surface step (2) prepared is modified is placed in 150 gram masses
Degree is in the copper sulphate pentahydrate aqueous solution of 4.5%, and after soaking 15 minutes at 40 DEG C, adding 150 gram mass concentration is
4.5% sodium thiosulfate solution, is warming up to 80 DEG C and reacts 1.0 hours, rinses with water, dries after taking out fiber
After obtain cuprous sulfide/glass fibre composite conducting fiber, the electrical conductivity of fiber is 9.1 × 10-1S/cm。
Embodiment 6
The present invention proposes the preparation method of a kind of electroconductive glass fibre, the steps include:
(1) alkali-free glass fibre that 20 grams clean up being immersed in 250 grams of concentration is the hydrochloric acid water of 2.0mol/L
In solution, soak 1 hour in 40 DEG C, after immersion, fully rinse with water, obtain hydroxylating glass after drying
Glass fiber;
(2) hydroxylating glass fibre prepared by step (1) is immersed the poly-second that 400 gram mass concentration are 0.8%
In alkene imines aqueous solution, soak 5 hours at 80 DEG C, after immersion, fully rinse with water, obtain after drying
The glass fibre that polymine surface is modified;
(3) it is dense that the glass fibre that polymine surface step (2) prepared is modified is placed in 250 gram masses
Degree is in the copper sulphate pentahydrate aqueous solution of 9%, and after soaking 15 minutes at 40 DEG C, adding 450 gram mass concentration is 5%
Sodium thiosulfate solution, is warming up to 80 DEG C and reacts 1.5 hours, obtains after taking out fiber after water rinsing, drying
To cuprous sulfide/glass fibre composite conducting fiber, the electrical conductivity of fiber is 1.1 × 100S/cm。
Embodiment 7
The present invention proposes the preparation method of a kind of electroconductive glass fibre, the steps include:
(1) alkali-free glass fibre that 20 grams clean up being immersed in 250 grams of concentration is the hydrochloric acid water of 2.5mol/L
In solution, soak 1 hour in 35 DEG C, after immersion, fully rinse with water, obtain hydroxyl by after fiber drying
The glass fibre of base;
(2) hydroxylating glass fibre prepared by step (1) is immersed the poly-second that 400 gram mass concentration are 2.8%
In alkene imines aqueous solution, soak 5 hours at 85 DEG C, after immersion, fully rinse with water, by fiber drying
After obtain polymine surface modify glass fibre;
(3) glass fibre that polymine surface step (2) prepared is modified is placed in 250 gram mass concentration
Being in the copper sulphate pentahydrate aqueous solution of 3%, after soaking 15 minutes at 40 DEG C, adding 250 gram mass concentration is
3% sodium thiosulfate solution, is warming up to 80 DEG C and reacts 1.5 hours, rinses with water, dries after taking out fiber
After obtain cuprous sulfide/glass fibre composite conducting fiber, the electrical conductivity of fiber is 5.8 × 10-1S/cm。
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all in invention
Spirit and principle within, any modification, equivalent substitution and improvement etc. made, should be included in the present invention
Protection domain within.
Claims (3)
1. the preparation method of an electroconductive glass fibre, it is characterised in that the steps include:
(1) alkali-free glass fibre is immersed in aqueous hydrochloric acid solution in 20 DEG C~50 DEG C immersions 0.5~2 hour,
After immersion, fully rinse with water, obtain hydroxylating glass fibre after drying;
(2) the hydroxylating glass fibre that step (1) obtains is immersed in the polyethylene that concentration is 0.5%~2%
In imines aqueous solution, soak 2~6 hours at 60 DEG C~90 DEG C, after immersion, fully rinse with water, do
The glass fibre that polymine surface is modified is obtained after dry;
(3) glass fibre that polymine surface step (2) obtained is modified is placed in mass concentration and is
In 2.5%~10% copper sulphate pentahydrate aqueous solution, after soaking 5~30 minutes at 20 DEG C~60 DEG C, add quality dense
Degree is 2.5%~5% sodium thiosulfate solution, is warming up to 75 DEG C~90 DEG C and reacts 0.3~1.5 hour, after taking-up
Cuprous sulfide/glass fibre composite conducting fiber is obtained after water rinsing, drying.
The preparation method of electroconductive glass fibre the most according to claim 1, it is characterised in that: described step (1)
Middle aqueous hydrochloric acid solution concentration is 1mol/L~3mol/.
The preparation method of electroconductive glass fibre the most according to claim 1, it is characterised in that: described step (3)
Middle copper sulphate pentahydrate aqueous solution is 1:1~1:2 with the mass ratio of sodium thiosulfate solution.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107902888A (en) * | 2017-11-21 | 2018-04-13 | 安徽玉然经编科技有限公司 | A kind of processing method for improving glass fibre electric conductivity |
CN109626658A (en) * | 2019-01-24 | 2019-04-16 | 黄河水利职业技术学院 | A kind of processing method of copper-contained electroplating waste water |
CN112010572A (en) * | 2020-08-17 | 2020-12-01 | 泰山玻璃纤维有限公司 | Conductive glass fiber and preparation method thereof |
CN113698143A (en) * | 2021-09-26 | 2021-11-26 | 武汉工程大学 | Semi-flexible asphalt mixture filled with metakaolin-based polymer and preparation method thereof |
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CN1030268A (en) * | 1987-07-01 | 1989-01-11 | 徐文治 | Cuprous sulfide conducting polypropylene nitrile fiber, yarn, knitting wool and preparation method |
GB2210069A (en) * | 1987-09-17 | 1989-06-01 | Courtaulds Plc | Electrically conductive cellulosic fibres |
CN101660264A (en) * | 2009-09-11 | 2010-03-03 | 北京化工大学 | Method for preparing polyimide/silver composite conductive fiber |
CN104805684A (en) * | 2015-04-21 | 2015-07-29 | 常熟市翔鹰特纤有限公司 | Manufacture method of conductive fire-retardant acrylic fiber |
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2016
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1030268A (en) * | 1987-07-01 | 1989-01-11 | 徐文治 | Cuprous sulfide conducting polypropylene nitrile fiber, yarn, knitting wool and preparation method |
GB2210069A (en) * | 1987-09-17 | 1989-06-01 | Courtaulds Plc | Electrically conductive cellulosic fibres |
CN101660264A (en) * | 2009-09-11 | 2010-03-03 | 北京化工大学 | Method for preparing polyimide/silver composite conductive fiber |
CN104805684A (en) * | 2015-04-21 | 2015-07-29 | 常熟市翔鹰特纤有限公司 | Manufacture method of conductive fire-retardant acrylic fiber |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107902888A (en) * | 2017-11-21 | 2018-04-13 | 安徽玉然经编科技有限公司 | A kind of processing method for improving glass fibre electric conductivity |
CN109626658A (en) * | 2019-01-24 | 2019-04-16 | 黄河水利职业技术学院 | A kind of processing method of copper-contained electroplating waste water |
CN112010572A (en) * | 2020-08-17 | 2020-12-01 | 泰山玻璃纤维有限公司 | Conductive glass fiber and preparation method thereof |
CN113698143A (en) * | 2021-09-26 | 2021-11-26 | 武汉工程大学 | Semi-flexible asphalt mixture filled with metakaolin-based polymer and preparation method thereof |
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Effective date of registration: 20230117 Address after: 024000 No. 6, Yiwei Road, Chifeng Hongshan High-tech Industrial Park, Hongshan District, Chifeng City, Inner Mongolia Autonomous Region Patentee after: Chifeng Bosite New Latitude Glass Fiber Manufacturing Co.,Ltd. Address before: 450007 No.1 Huaihe Road, Xinzheng Shuanghu Economic and Technological Development Zone, Zhengzhou, Henan Province Patentee before: ZHONGYUAN University OF TECHNOLOGY |