CN114933424A - High silica glass fiber continuous yarn coating material and preparation method thereof - Google Patents

High silica glass fiber continuous yarn coating material and preparation method thereof Download PDF

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Publication number
CN114933424A
CN114933424A CN202210591450.7A CN202210591450A CN114933424A CN 114933424 A CN114933424 A CN 114933424A CN 202210591450 A CN202210591450 A CN 202210591450A CN 114933424 A CN114933424 A CN 114933424A
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high silica
continuous yarn
silica glass
yarn
container
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贺广东
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Jiangsu Hengzhou Special Glass Fibers Co ltd
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Jiangsu Hengzhou Special Glass Fibers Co ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10Coating
    • C03C25/465Coatings containing composite materials
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10Coating
    • C03C25/24Coatings containing organic materials
    • C03C25/26Macromolecular compounds or prepolymers
    • C03C25/32Macromolecular compounds or prepolymers obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
    • C03C25/36Epoxy resins

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Organic Chemistry (AREA)
  • Composite Materials (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Surface Treatment Of Glass Fibres Or Filaments (AREA)

Abstract

The invention discloses a high silica glass fiber continuous yarn coating material and a preparation method thereof, wherein the high silica glass fiber continuous yarn coating material is composed of 0.08-0.2% of glacial acetic acid, 0.2-1.0% of coupling agent, 0.2-1.0% of emulsifier, 1.0-2.0% of epoxy resin, 0.08-0.2% of wetting agent, 0.08-0.2% of antistatic agent and 95.4-98.36% of purified water. After the continuous yarn is coated with the coating material, the strength of the high silica glass continuous yarn reaches more than 6 times of that of the yarn before coating, the yarn strength is measured to be as high as 0.54N/tex, the yarn strength is improved, the yarn surface is smooth, and the technical problem that the high silica glass continuous yarn cannot be woven or knitted is solved.

Description

High silica glass fiber continuous yarn coating material and preparation method thereof
Technical Field
The invention belongs to the technical field of high silica glass fiber yarn preparation, and particularly relates to a high silica glass fiber continuous yarn coating material and a preparation method thereof.
Background
The high silica fiber is a short name of high-purity silicon oxide amorphous continuous fiber, the silicon oxide content of the high silica fiber is 96-98%, and the high silica fiber can continuously resist the temperature of 1000 ℃ and can temporarily resist the temperature of 1400 ℃; the finished product mainly comprises continuous yarn, rope belt, sleeve, screen cloth and stitch-bonded product, is mainly applied to the fire prevention and heat insulation at the ultra-high temperature of 1000 ℃, has the diameter of a single fiber of more than 5 microns, does not contain any asbestos or ceramic cotton, and is completely harmless to the health of human body.
The high silica fiber can keep good strength and elasticity for a long time at 1000 ℃, and is an effective heat barrier for ultrahigh-temperature heat flow and jet flame and a reliable protection device for personnel facilities; the high-temperature resistant alloy has low heat conductivity coefficient, has good resistance to high-temperature impact, is inert to most chemicals, has good corrosion resistance to compounds at high temperature, corrosive minerals and weakly alkaline molten alloy, and can normally and continuously work under the conditions of high heat and strong radiation.
In the production, the high silica fiber continuous yarn is formed by drawing, untwisting and twisting high silica glass balls to form the high silica fiber continuous yarn (base yarn) with the silica content of 66-68%, then hydrochloric acid leaching is carried out, and phase separation of the structure is utilized to lead B to be separated from B 2 0 3 And Na 2 Leaching out O component and transferring into solution to make Si0 2 Obtaining a microporous silica framework with the enrichment of more than 96 percent to obtain high silica fiber yarn with the silica content of more than 96 percent, performing high-temperature sintering and shaping at the temperature of 600-800 ℃ to close micropores generated by chemical reaction of the yarn in the acid leaching process to prepare high-performance high silica fiber continuous yarn, and finally performing integral soaking, coating and drying to obtain the high silica fiber continuous yarn; the high silica fiber continuous yarn can be used for a long time at 900 ℃, and is mainly used for the aspects of military industry, aerospace and the like.
Because the high silica yarn (base yarn) has low strength after acid leaching and high-temperature sintering, the strength of the actually tested yarn is 0.05-0.08N/tex on average, and the yarn can only be used as an ablation-resistant material and cannot be suitable for weaving or knitting fabrics. In order to use the high silica continuous yarn for weaving, some manufacturers coat the high silica continuous yarn with various coating materials to improve the strength of the yarn, and most of the coating materials are polytetrafluoroethylene emulsion. If the leached impurities in the acid leaching process of the high-silica continuous yarn are not cleaned, the sintered yarn has basically no strength at the positions which are not cleaned, the yarn still has no strength after being coated, and breakpoints exist in the later use process of the yarn, so that the yarn is broken.
Disclosure of Invention
Aiming at the problem of low strength of high silica continuous yarn provided by the background technology, the invention researches and designs a high silica glass fiber continuous yarn coating material and a preparation method thereof, and aims to: provides a coating material for greatly improving the strength of high-silica continuous yarns and a preparation method thereof.
The technical solution of the invention is as follows:
a high silica glass fiber continuous yarn coating material comprises 0.08-0.2% of glacial acetic acid, 0.2-1.0% of coupling agent, 0.2-1.0% of emulsifier, 1.0-2.0% of epoxy resin, 0.08-0.2% of wetting agent, 0.08-0.2% of antistatic agent and 95.4-98.36% of purified water in percentage by weight.
The preparation process of the high silica glass fiber continuous yarn comprises the following steps: adding the high silica glass balls into a crucible, melting and drawing at 1350 ℃ to form high silica protofilaments, and untwisting and twisting the high silica protofilaments by a twisting machine to form high silica fiber continuous yarns (base yarns); then leaching the high silica fiber continuous yarn by hydrochloric acid to obtain the high silica fiber yarn with the silica content of more than 96%; then performing high-temperature sintering and shaping at the temperature of 800 ℃ through 600 plus materials to obtain sintered high-silica fiber continuous yarns; and soaking and coating the sintered high silica fiber continuous yarn in the coating liquid for 60min, taking out the yarn, and drying in a drying room at 80 ℃ to obtain the high silica glass fiber continuous yarn with high strength.
The linear density of the high silica protofilament is 32tex, the density of the high silica continuous yarn is 288tex, the density of the high silica fiber continuous yarn is 240tex, and the density of the sintered continuous yarn is 220 tex.
The high silica glass ball contains SiO 2 66-68% of Na 2 O is 7-8%, B 2 O 3 22-23% of Al 2 O 3 1-5 percent of the total weight percentage.
The coupling agent is an A-1100 coupling agent.
The emulsifier is EL-80 emulsifier.
The epoxy resin is NBR-290 epoxy resin.
The wetting agent is NBR-1280 wetting agent.
The antistatic agent is an NBS-900 antistatic agent.
A preparation method of a high silica glass fiber continuous yarn coating material comprises the following steps:
(1) weighing the purified water, putting the purified water into a clean container, starting a stirring device, and stirring at the speed of 100 rpm;
(2) weighing glacial acetic acid, and slowly adding the glacial acetic acid into the container in the step (1) in a streamline shape;
(3) weighing a coupling agent, adding the coupling agent into the container in the step (1), and stirring for 30 min;
(4) weighing an emulsifier and adding the emulsifier into the container in the step (3);
(5) weighing epoxy resin, putting the epoxy resin into another container, adding purified water with the temperature of 80-100 ℃ into the container for melting, adding the completely melted epoxy resin into a plastic barrel, washing the other container with purified water, and adding the washing water into the container in the step (4);
(6) weighing a wetting agent and continuously adding the wetting agent into the container in the step (4);
(7) weighing an antistatic agent and continuously adding the antistatic agent into the container in the step (4);
(8) and (4) adding purified water into the container in the step (4), continuing stirring for 30min, and stopping stirring to obtain the high silica glass fiber continuous yarn coating material.
The invention has the beneficial effects that: glacial acetic acid added into the coating material is weakly acidic, is used for adjusting the pH value of the coating liquid, is used for neutralizing an alkaline coupling agent, and is beneficial to hydrolysis of the coupling agent; a-1100 coupling agent, the silicon-containing part in the molecule can repair the strong bond of the base material, and the tensile breaking strength of the yarn is improved; the amine functional group in the molecule can react with the emulsifier and the epoxy resin in the coating liquid to increase the binding force of the coating liquid on the surface of the continuous yarn; the emulsifier is EL-80 emulsifier, has unique emulsification, can effectively improve the emulsification of the coating solution, and can increase the smoothness and softness of the continuous yarn; the epoxy resin is NBR-290 epoxy resin which is used as a binder, and a layer of protective film is formed on the surface of the yarn after drying, so that the strength of the continuous yarn can be improved; the wetting agent is an NBR-1280 wetting agent and is used for improving the surface tension and permeability of the coating and leading the coating to be capable of wetting continuous yarns better so as to improve the adhesive force of the coating liquid; the antistatic agent is NBS-900 antistatic agent and reduces continuous yarnSurface resistivitySo as to achieve the antistatic purpose.
After the continuous yarn is coated with the coating material, the strength of the high silica glass continuous yarn reaches more than 6 times of that of the yarn before coating, the yarn strength is measured to be as high as 0.54N/tex, the yarn strength is improved, the yarn surface is smooth, and the technical problem that the high silica glass continuous yarn cannot be woven or knitted is solved.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
The preparation process of the high silica glass fiber continuous yarn coating material comprises the following steps:
(1) weighing 50kg of purified water, putting the purified water into a clean container, starting a stirring device, and stirring at the speed of 100 rpm;
(2) weighing 80g of glacial acetic acid, and slowly adding the glacial acetic acid into the container in the step (1) in a streamline shape;
(3) weighing 200g of A-1100 coupling agent, adding into the container in the step (1), and stirring for 30 min;
(4) weighing 200g of EL-80 emulsifier, and adding into the container in the step (3);
(5) weighing 1000g of NBR-290 epoxy resin, putting the NBR-290 epoxy resin into another container, adding 2kg of purified water with the temperature of 80-100 ℃ into the container for melting, adding the completely melted epoxy resin into the container in the step (4), washing the other container with 2kg of purified water, and adding the washing water into the container in the step (4);
(6) weighing 80g of NBR-1280 wetting agent, and adding into the container in the step (4);
(7) weighing 80g of NBS-900 antistatic agent, and adding into the container in the step (4);
(8) adding 44.36kg of purified water into the container in the step (4) to ensure that the total weight of the coating liquid is 100 kg;
(9) and after stirring is continued for 30min, stopping stirring, and thus finishing the preparation of the high silica glass fiber continuous yarn coating material.
Coating high silica matrix glassGlass ball (SiO component content) 2 66-68% of Na 2 O is 7-8%, B 2 O 3 22-23% of Al 2 O 3 1-5%) is added into a crucible, melted at 1350 ℃ and drawn into silica precursor with the linear density of 32tex, the silica precursor with the linear density of 32tex is untwisted and twisted by a twisting machine to form silica continuous yarn with the linear density of 288tex, the silica continuous yarn with the linear density of 288tex is leached by hydrochloric acid, and Na in the yarn components 2 O and B 2 O 3 Separating phase in hydrochloric acid, leaching all the solution into hydrochloric acid solution, washing with water, and washing hydrochloric acid and other impurities in the yarn to obtain SiO 2 High silica fiber continuous yarn with the content of more than 96% and the linear density of 240 tex; putting the 240tex continuous yarn into a 600-800 ℃ high-temperature sintering furnace for heat sintering and shaping treatment to prepare 220tex sintered continuous yarn (at the moment, the yarn strength test is 0.05-0.08N/tex on average); and (3) soaking and coating the 220tex sintered continuous yarn in the high silica glass fiber continuous yarn coating material for 60min, taking out, and drying in a drying room at 80 ℃ to obtain the high silica glass fiber continuous yarn with high strength (the yarn strength is more than 0.4N/tex on average).
Example 2
The preparation process of the high silica glass fiber continuous yarn coating material comprises the following steps:
(1) weighing 50kg of purified water, putting the purified water into a clean container, starting a stirring device, and stirring at the speed of 100 rpm;
(2) weighing 200g of glacial acetic acid, and slowly adding the glacial acetic acid into the container in the step (1) in a streamline shape;
(3) weighing 1000g of A-1100 coupling agent, adding into the container in the step (1), and stirring for 30 min;
(4) weighing 1000g of EL-80 emulsifier, and adding into the container in the step (3);
(5) weighing 2000g of NBR-290 epoxy resin into another container, adding 2kg of purified water with the temperature of 80-100 ℃ into the container for melting, adding the completely melted epoxy resin into the container in the step (4), washing the other container with 2kg of purified water, and adding the washing water into the container in the step (4); (ii) a
(6) Weighing 200g of NBR-1280 wetting agent, and adding the NBR-1280 wetting agent into the container in the step (4);
(7) weighing 200g of NBS-900 antistatic agent and adding into the container in the step (4);
(8) adding 41.4kg of purified water into the container in the step (4) to ensure that the total weight of the coating liquid is 100 kg;
(9) continuing stirring for 30min, and stopping stirring; thus, the preparation of the high silica glass fiber continuous yarn coating material is completed.
High silica matrix glass spheres (with the component content of SiO) 2 66-68% of Na 2 O is 7-8%, B 2 O 3 22-23% of Al 2 O 3 1-5%) is added into a crucible, melted at 1350 ℃ and drawn into silica precursor with the linear density of 32tex, the silica precursor with the linear density of 32tex is untwisted and twisted by a twisting machine to form silica continuous yarn with the linear density of 288tex, the silica continuous yarn with the linear density of 288tex is leached by hydrochloric acid, and Na in the yarn components 2 O and B 2 O 3 Separating phase in hydrochloric acid, leaching all the solution into hydrochloric acid solution, washing with water, and washing hydrochloric acid and other impurities in the yarn to obtain SiO 2 High silica fiber continuous yarn with the content of more than 96% and the linear density of 240 tex; putting the 240tex continuous yarn into a 600-800 ℃ high-temperature sintering furnace for heat sintering and shaping treatment to prepare 220tex sintered continuous yarn (at the moment, the yarn strength test is 0.05-0.08N/tex on average); and (3) soaking and coating the 220tex sintered continuous yarn in the coating liquid for 60min, taking out, and then drying in a drying room at 80 ℃ to obtain the high silica glass fiber continuous yarn with high strength (at the moment, the strength test of the yarn is more than 0.5N/tex).
Example 3
The preparation process of the high silica glass fiber continuous yarn coating material comprises the following steps:
(1) weighing 50kg of purified water, putting the purified water into a clean container, starting a stirring device, and stirring at the speed of 100 rpm;
(2) weighing 140g of glacial acetic acid, and slowly adding the glacial acetic acid into the container in the step (1) in a streamline shape;
(3) weighing 600g of A-1100 coupling agent, adding into the container in the step (1), and stirring for 30 min;
(4) weighing 600g of EL-80 emulsifier, and adding into the container in the step (3);
(5) weighing 1500g of NBR-290 epoxy resin into another container, adding 2kg of purified water with the temperature of 80-100 ℃ into the container for melting, adding the completely melted epoxy resin into the container in the step (4), washing the other container with 2kg of purified water, and adding the washing water into the container in the step (4);
(6) weighing 140g of NBR-1280 wetting agent and adding the NBR-1280 wetting agent into the container in the step (4);
(7) weighing 140g of NBS-900 antistatic agent and adding into the container in the step (4);
(8) adding 42.88kg of purified water into the container in the step (4) to ensure that the total weight of the coating liquid is 100 kg;
(9) continuing stirring for 30min, and stopping stirring; to this end, the coating emulsion formulation is complete.
High silica matrix glass spheres (with the component content of SiO) 2 66-68% of Na 2 O is 7-8%, B 2 O 3 22-23% of Al 2 O 3 1-5%) is added into a crucible, melted at 1350 ℃ and drawn into silica precursor with the linear density of 32tex, the silica precursor with the linear density of 32tex is untwisted and twisted by a twisting machine to form silica continuous yarn with the linear density of 288tex, the silica continuous yarn with the linear density of 288tex is leached by hydrochloric acid, and Na in the yarn components 2 O and B 2 O 3 Separating phase in hydrochloric acid, leaching all the solution into hydrochloric acid solution, washing with water, and washing hydrochloric acid and other impurities in the yarn to obtain SiO 2 High silica fiber continuous yarn with content of more than 96% and linear density of 240 tex; putting the 240tex continuous yarn into a 600-800 ℃ high-temperature sintering furnace for heat sintering and shaping treatment to prepare 220tex sintered continuous yarn (at the moment, the yarn strength test is 0.05-0.08N/tex on average); and (3) soaking and coating the 220tex sintered continuous yarn in the coating liquid for 60min, taking out, and then drying in a drying room at 80 ℃ to obtain the high silica glass fiber continuous yarn with high strength (at the moment, the strength test of the yarn is more than 0.45N/tex).
The high silica glass fiber continuous yarn coated with the coating material of the present invention in examples 1 to 3 and the high silica glass fiber yarn not coated with the coating material of the present invention were respectively subjected to performance tests as comparative examples, and the test results are shown in table 1.
Table 1 comparative table of the performance tests of continuous yarns of high-silica glass fibres coated with a coating according to the invention and uncoated
Figure BDA0003665332630000061
The case of particularly low strength, which occurs in the test strength, is treated as an abnormal case, the main reason for which is that the coating solution cannot effectively repair and increase the strength of weak spots, which are caused by the yarn before coating.
As can be seen from Table 1, after the high silica glass fiber continuous yarn is coated with the coating material, the strength of the high silica glass continuous yarn is more than 6 times of that of the yarn before coating, the yarn strength is actually measured to be 0.54N/tex, the yarn strength is improved, the yarn surface is smooth, and the technical problem that the high silica glass continuous yarn cannot be woven or knitted is solved.
The above examples merely illustrate specific embodiments of the present disclosure, but embodiments of the present disclosure are not limited by the above. Any changes, modifications, substitutions, combinations, and simplifications which do not materially depart from the spirit and principles of the inventive concepts disclosed herein are intended to be equivalent permutations and to be included within the scope of the invention as defined by the following claims.

Claims (10)

1. A high silica glass fiber continuous yarn coating material is characterized in that: the antistatic agent is composed of 0.08-0.2% of glacial acetic acid, 0.2-1.0% of coupling agent, 0.2-1.0% of emulsifier, 1.0-2.0% of epoxy resin, 0.08-0.2% of wetting agent, 0.08-0.2% of antistatic agent and 95.4-98.36% of purified water by weight percentage.
2. The high silica glass fiber continuous yarn coating of claim 1, wherein: the preparation process of the high silica glass fiber continuous yarn comprises the following steps: adding the high silica glass balls into a crucible, melting and drawing at 1350 ℃ to form high silica protofilaments, and untwisting and twisting the high silica protofilaments by a twisting machine to form high silica fiber continuous yarns (base yarns); then leaching the high silica fiber continuous yarn by hydrochloric acid to obtain the high silica fiber yarn with the silica content of more than 96%; then performing high-temperature sintering and shaping at the temperature of 800 ℃ through 600 plus materials to obtain sintered high-silica fiber continuous yarns; and soaking and coating the sintered high silica fiber continuous yarn in the coating liquid for 60min, taking out the yarn, and drying in a drying room at 80 ℃ to obtain the high silica glass fiber continuous yarn with high strength.
3. The high silica glass fiber continuous yarn coating of claim 2, wherein: the linear density of the high silica protofilament is 32tex, the density of the high silica continuous yarn is 288tex, the density of the high silica fiber continuous yarn is 240tex, and the density of the sintered continuous yarn is 220 tex.
4. The high silica glass fiber continuous yarn coating of claim 2, wherein: the high silica glass ball contains SiO 2 66-68% of Na 2 O is 7-8%, B 2 O 3 22-23% of Al 2 O 3 1-5 percent of the total weight percentage.
5. The high silica glass fiber continuous yarn coating of claim 1, wherein: the coupling agent is an A-1100 coupling agent.
6. The high silica glass fiber continuous yarn coating of claim 1, wherein: the emulsifier is EL-80 emulsifier.
7. The high silica glass fiber continuous yarn coating of claim 1, wherein: the epoxy resin is NBR-290 epoxy resin.
8. The high silica glass fiber continuous strand coating of claim 1, wherein: the wetting agent is NBR-1280 wetting agent.
9. The high silica glass fiber continuous yarn coating of claim 1, wherein: the antistatic agent is an NBS-900 antistatic agent.
10. A method of making a high silica glass fiber continuous strand coating of claim 1, wherein: the method comprises the following steps:
(1) weighing the purified water, putting the purified water into a clean container, starting a stirring device, and stirring at the speed of 100 rpm;
(2) weighing glacial acetic acid, and slowly adding the glacial acetic acid into the container in the step (1) in a streamline shape;
(3) weighing a coupling agent, adding the coupling agent into the container in the step (1), and stirring for 30 min;
(4) weighing an emulsifier and adding the emulsifier into the container in the step (3);
(5) weighing epoxy resin and putting the epoxy resin into another container, adding purified water with the temperature of 80-100 ℃ into the container for melting, adding the completely melted epoxy resin into a plastic barrel, washing the other container by using the purified water, and adding the washing water into the container in the step (4);
(6) weighing a wetting agent and continuously adding the wetting agent into the container in the step (4);
(7) weighing an antistatic agent and continuously adding the antistatic agent into the container in the step (4);
(8) and (4) adding purified water into the container in the step (4), continuing stirring for 30min, and stopping stirring to obtain the high silica glass fiber continuous yarn coating material.
CN202210591450.7A 2022-05-27 2022-05-27 High silica glass fiber continuous yarn coating material and preparation method thereof Pending CN114933424A (en)

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Cited By (1)

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CN115477481A (en) * 2022-09-14 2022-12-16 重庆海科保温材料有限公司 Mineral oil for glass wool products and preparation method thereof

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CN102992649A (en) * 2012-12-19 2013-03-27 江苏九鼎新材料股份有限公司 Process of binary component high-silica glass fiber wetting agent
CN112341008A (en) * 2020-10-25 2021-02-09 陕西华特新材料股份有限公司 High silica glass fiber continuous yarn coating composite material and preparation method thereof

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CN102992649A (en) * 2012-12-19 2013-03-27 江苏九鼎新材料股份有限公司 Process of binary component high-silica glass fiber wetting agent
CN112341008A (en) * 2020-10-25 2021-02-09 陕西华特新材料股份有限公司 High silica glass fiber continuous yarn coating composite material and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115477481A (en) * 2022-09-14 2022-12-16 重庆海科保温材料有限公司 Mineral oil for glass wool products and preparation method thereof

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