CN106948176A - A kind of silicon nitride fiber sizing agent and preparation method thereof - Google Patents

A kind of silicon nitride fiber sizing agent and preparation method thereof Download PDF

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Publication number
CN106948176A
CN106948176A CN201710182433.7A CN201710182433A CN106948176A CN 106948176 A CN106948176 A CN 106948176A CN 201710182433 A CN201710182433 A CN 201710182433A CN 106948176 A CN106948176 A CN 106948176A
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China
Prior art keywords
sizing agent
silicon nitride
parts
nitride fiber
fiber sizing
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CN201710182433.7A
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Chinese (zh)
Inventor
包海峰
黄晓
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WUHAN LOONGTOP NEW MATERIAL TECHNOLOGY Co Ltd
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WUHAN LOONGTOP NEW MATERIAL TECHNOLOGY Co Ltd
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Priority to CN201710182433.7A priority Critical patent/CN106948176A/en
Publication of CN106948176A publication Critical patent/CN106948176A/en
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/55Epoxy resins
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/11Compounds containing epoxy groups or precursors thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53Polyethers

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The present invention proposes a kind of silicon nitride fiber sizing agent, includes by weight:5 15 parts of main slurry;15 parts of emulsifying agent;0.1 1 parts of lubricant;80 95 parts of deionized water.On the one hand hydrophily is improved using epoxy resin in the present invention, the emulsion for the stabilization for being dissolved in water is formed;On the other hand diglycidyl ether is added, the polymer of formation improves the interface characteristics of sizing agent, the external force that matrix is born passes to enhancing phase, play the function served as bridge between matrix and enhancing phase, the intensity and pliability of synnema are improved, can also increase its adhesion prevents that fiber surface from producing lousiness and fracture of wire phenomenon.The sizing agent adhesion strength is high, and overall performance is stable, without any volatile organic matter, is conducive to the protection of environment.

Description

A kind of silicon nitride fiber sizing agent and preparation method thereof
Technical field
The present invention relates to a kind of silicon nitride fiber sizing agent and preparation method thereof.
Background technology
Silicon nitride fiber is wide because of its superior performance in the performance such as mechanical property, heat endurance, resistance to oxidation, corrosion-resistant It is general to be applied to the fields such as petrochemical industry, automobile engine, electron electric power, Aero-Space and nuclear industry.With by organosilicon polymer Prepare silicon carbide fibre similar, silicon nitride fiber can also be prepared using the converting method of preceramic polymer, i.e., by poly- silicon nitrogen The polymer such as alkane, polycarbosilazanes are constituted through synthesis, spinning, cure treatment and the step preparation section of high temperature sintering 4.
Compared to developed countries such as the U.S., Japan, France, exploitation of the China to silicon nitride fiber is started late.In fiber Commercial process in be very easy to produce synnema and rub, so as to cause the generation of a large amount of lousiness, had a strong impact on fibre Being smoothed out for continuous production is tieed up, so starching processing must be carried out to silicon nitride fiber surface.Starching processing can be simple Ground is understood as coating layer protecting film on silicon nitride fiber surface, and the main function of this tunic is:(1) moisture in air is avoided Or pollution of other impurity to silicon nitride fiber surface;(2) make silicon nitride fiber boundling, improve its processing performance;(3) nitrogen is reduced The interfibrous friction of SiClx, reduction lousiness and fracture of wire phenomenon, (4) improve the intensity of silicon nitride fiber, improve the quality of product.
In the production of country variant silicon nitride fiber, the technique of starching is similar, but the Ju Ti Pei Fang of sizing agent belongs to Top trade secret, it is difficult to the formula of sizing agent and relevant information of offshore company are found, and both at home and abroad on carbon fiber sizing agent Document it is but relatively many.It can make carbon fiber that there is pliability as Japanese this grease of bamboo company develops one kind, and it is fine to improve carbon The sizing agent of wearability is tieed up, it can effectively suppress the generation of filoplume phenomenon, control the fracture of synnema;Zhang Xiping etc. is in epoxy Serial emulsifying agent of alkyl phenol etc. is added in resin and is configured to emulsion pasting agent, as a result shows that the interlayer of material after being handled through starching is cut Shearing stress substantially increases;Li Yang etc. have developed the sizing agent of the epoxy resin that is modified using oleamide as main component;Yu Mu Fire etc. reports a kind of epoxy resin sizing agent of carbon nano-tube modification;Zhang Zhi is modest etc., and to develop a kind of Epoxy/Nano SiO2 miscellaneous Change sizing agent.
Compared with carbon fiber, silicon nitride fiber diameter prepared by the converting method of preceramic polymer is bigger, for fiber The gathering of synnema, the arrangement difficulty of lousiness are also bigger, therefore requirement of the silicon nitride fiber to sizing agent is then higher tightened up.
The content of the invention
In order to overcome the deficiencies in the prior art, the present invention proposes a kind of environment-friendly silicon nitride fiber sizing agent, should Sizing agent adhesion strength is high, and overall performance is stable.On the one hand hydrophily is improved using epoxy resin in the present invention, formation is dissolved in water Stabilization emulsion;On the other hand diglycidyl ether is added, the polymer of formation improves the interface characteristics of sizing agent, and matrix is held The external force received passes to enhancing phase, plays the function served as bridge between matrix and enhancing phase, improves the intensity and pliability of synnema, Its adhesion, which can be increased, prevents that fiber surface from producing lousiness and fracture of wire phenomenon.
The technical proposal of the invention is realized in this way:
A kind of silicon nitride fiber sizing agent, includes by weight:5-15 parts of main slurry;1-5 parts of emulsifying agent;Lubricant 0.1-1 parts;80-95 parts of deionized water.
Preferably, described main slurry is the mixture of epoxy resin and diglycidyl ether, and its weight ratio is 3:1~1: 1。
Preferably, described epoxy resin is bisphenol A type epoxy resin E51.
Preferably, described emulsifying agent is nonionic surface active agent:Tween-40.
Preferably, described lubricant is polyethylene glycol laurate.
A kind of preparation method of silicon nitride fiber sizing agent, comprises the following steps:
(1) by the epoxy resin of 5-15 parts by weight and diglycidyl ether by weight 3:1~1:1 mixing, at 60 DEG C 5min is stirred with 800r/min, it is well mixed and system A is made;
(2) 1-5 parts by weight Emulsifier and 0.1-1 parts by weight lubricants are added in said mixture system A, 60 DEG C with System B is made in 1000r/min stirrings more than 30min;
(3) 40 DEG C with the emulsification of 5000r/min high rotating speed cutting under toward being slowly added to 80- with separatory funnel in system B The deionized water of 95 parts by weight, with the increase of rate of water added, system phase inversion adds water in 60min and continued after finishing with 800r/min 20min is stirred until forming uniform and stable emulsion, silicon nitride fiber sizing agent is obtained after cooling.
What the present invention was produced has the beneficial effect that:(1) present invention is a kind of aqueous epoxy emulsion type silicon nitride fiber sizing agent, Its emulsifying process is simple, and raw material is easy to get and low cost.(2) sizing agent is conducive to environment without any volatile organic matter Protection.(3) sizing agent can effectively improve synnema intensity, reduce fiber surface lousiness and fracture of wire, with convergence it is good and The advantages of pliability is good.
Embodiment
Technical scheme is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that retouched The embodiment stated is only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, sheet The every other embodiment that field those of ordinary skill is obtained under the premise of creative work is not made, belongs to the present invention The scope of protection.
Embodiment 1
The preparation method of sizing agent comprises the following steps in the present embodiment:
(1) by 5 parts of bisphenol A type epoxy resin E51 and diglycidyl ether by weight 3:1 mixing, at 60 DEG C with 800r/min stirs 5min, is well mixed it and system A is made;
(2) in said mixture system A add 1 part of Tween-40 and 0.1 part of polyethylene glycol laurate, 60 DEG C with System B is made in 1000r/min stirrings more than 30min;
(3) 40 DEG C with the emulsification of 5000r/min high rotating speed cutting under toward being slowly added to 95 parts with separatory funnel in system B Deionized water, with the increase of rate of water added, system phase inversion adds water in 60min and continues to stir 20min with 800r/min after finishing Until forming uniform and stable emulsion, silicon nitride fiber sizing agent is obtained after cooling.
Embodiment 2
The preparation method of sizing agent comprises the following steps in the present embodiment:
(1) by 10 parts of epoxy resin E51 and diglycidyl ether by weight 2:1 mixing, with 800r/ at 60 DEG C Min stirs 5min, is well mixed it and system A is made;
(2) in said mixture system A add 3 parts of Tween-40 and 0.5 part of polyethylene glycol laurates, 60 DEG C with System B is made in 1000r/min stirrings more than 30min;
(3) 40 DEG C with the emulsification of 5000r/min high rotating speed cutting under toward being slowly added to 86.5 with separatory funnel in system B The deionized water of part, with the increase of rate of water added, system phase inversion is added water in 60min and continues to be stirred with 800r/min after finishing 20min is until the uniform and stable emulsion of formation, obtains silicon nitride fiber sizing agent after cooling.
Embodiment 3
The preparation method of sizing agent comprises the following steps in the present embodiment:
(1) by 15 parts of epoxy resin E51 and diglycidyl ether by weight 1:1 mixing, with 800r/ at 60 DEG C Min stirs 5min, is well mixed it and system A is made;
(2) in said mixture system A add 5 parts of Tween-40 and 1 part of polyethylene glycol laurates, 60 DEG C with System B is made in 1000r/min stirrings more than 30min;
(3) 40 DEG C with the emulsification of 5000r/min high rotating speed cutting under toward being slowly added to 80 parts with separatory funnel in system B Deionized water, with the increase of rate of water added, system phase inversion adds water in 60min and continues to stir 20min with 800r/min after finishing Until forming uniform and stable emulsion, silicon nitride fiber sizing agent is obtained after cooling.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, all essences in the present invention God is with principle, and any modifications, equivalent substitutions and improvements made etc. should be included within the scope of the present invention.

Claims (6)

1. a kind of silicon nitride fiber sizing agent, it is characterised in that include by weight:5-15 parts of main slurry;Emulsifying agent 1-5 Part;0.1-1 parts of lubricant;80-95 parts of deionized water.
2. a kind of silicon nitride fiber sizing agent as claimed in claim 1, it is characterised in that described main slurry is epoxy resin With the mixture of diglycidyl ether, its weight ratio is 3:1~1:1.
3. a kind of silicon nitride fiber sizing agent as claimed in claim 2, it is characterised in that described epoxy resin is bisphenol-A Type epoxy resin E51.
4. a kind of silicon nitride fiber sizing agent as claimed in claim 1, it is characterised in that described emulsifying agent is nonionic Surfactant:Tween-40.
5. a kind of silicon nitride fiber sizing agent as claimed in claim 1, it is characterised in that described lubricant is polyethylene glycol Laurate.
6. a kind of preparation method of silicon nitride fiber sizing agent, it is characterised in that comprise the following steps:
(1) by the epoxy resin of 5-15 parts by weight and diglycidyl ether by weight 3:1~1:1 mixing, at 60 DEG C with 800r/min stirs 5min, is well mixed it and system A is made;
(2) 1-5 parts by weight Emulsifier and 0.1-1 parts by weight lubricants are added in said mixture system A, 60 DEG C with System B is made in 1000r/min stirrings more than 30min;
(3) 40 DEG C with the emulsification of 5000r/min high rotating speed cutting under weigh toward being slowly added to 80-95 with separatory funnel in system B The deionized water of part is measured, with the increase of rate of water added, system phase inversion is added water in 60min and continues to be stirred with 800r/min after finishing 20min is until the uniform and stable emulsion of formation, obtains silicon nitride fiber sizing agent after cooling.
CN201710182433.7A 2017-03-24 2017-03-24 A kind of silicon nitride fiber sizing agent and preparation method thereof Pending CN106948176A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107620208A (en) * 2017-09-27 2018-01-23 中国人民解放军国防科技大学 Nitride fiber impregnating compound and coating method thereof
CN108755123A (en) * 2018-05-15 2018-11-06 天津工业大学 A kind of silicon nitride fiber surface conditioning agent and preparation method thereof
CN110184821A (en) * 2019-05-05 2019-08-30 宜兴市新立织造有限公司 A kind of alumina fibre flexible modifying agent and preparation method thereof
CN110305464A (en) * 2019-07-05 2019-10-08 天津工业大学 A kind of continuous nitride silica fibre reinforced resin base composite wire and preparation method thereof
CN114855458A (en) * 2022-06-17 2022-08-05 福建立亚新材有限公司 A kind of oil for remediating wear wave-transmitting silicon nitride fiber and preparation method thereof
CN115182162A (en) * 2022-07-21 2022-10-14 武汉纺织大学 Preparation method and application method of special sizing agent for nitride fibers

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JPH07166475A (en) * 1993-12-14 1995-06-27 Sumitomo Chem Co Ltd Alumina fiber with sizing agent
CN103572608A (en) * 2012-08-10 2014-02-12 江苏恒神纤维材料有限公司 Water-based epoxy emulsion type carbon fiber sizing agent and preparation method thereof
CN105064030A (en) * 2015-08-19 2015-11-18 国网智能电网研究院 Carbon fiber sizing agent and preparation method thereof

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CN103572608A (en) * 2012-08-10 2014-02-12 江苏恒神纤维材料有限公司 Water-based epoxy emulsion type carbon fiber sizing agent and preparation method thereof
CN105064030A (en) * 2015-08-19 2015-11-18 国网智能电网研究院 Carbon fiber sizing agent and preparation method thereof

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107620208A (en) * 2017-09-27 2018-01-23 中国人民解放军国防科技大学 Nitride fiber impregnating compound and coating method thereof
CN107620208B (en) * 2017-09-27 2019-07-19 中国人民解放军国防科技大学 Nitride fiber impregnating compound and coating method thereof
CN108755123A (en) * 2018-05-15 2018-11-06 天津工业大学 A kind of silicon nitride fiber surface conditioning agent and preparation method thereof
CN110184821A (en) * 2019-05-05 2019-08-30 宜兴市新立织造有限公司 A kind of alumina fibre flexible modifying agent and preparation method thereof
CN110184821B (en) * 2019-05-05 2022-02-11 宜兴市新立织造有限公司 Alumina fiber flexible modifier and preparation method thereof
CN110305464A (en) * 2019-07-05 2019-10-08 天津工业大学 A kind of continuous nitride silica fibre reinforced resin base composite wire and preparation method thereof
CN114855458A (en) * 2022-06-17 2022-08-05 福建立亚新材有限公司 A kind of oil for remediating wear wave-transmitting silicon nitride fiber and preparation method thereof
CN115182162A (en) * 2022-07-21 2022-10-14 武汉纺织大学 Preparation method and application method of special sizing agent for nitride fibers
CN115182162B (en) * 2022-07-21 2023-12-22 武汉纺织大学 Preparation method and application method of a special sizing agent for nitride fibers

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Application publication date: 20170714