CN106894238A - A kind of silicon carbide fibre sizing agent and preparation method thereof - Google Patents
A kind of silicon carbide fibre sizing agent and preparation method thereof Download PDFInfo
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- CN106894238A CN106894238A CN201710182431.8A CN201710182431A CN106894238A CN 106894238 A CN106894238 A CN 106894238A CN 201710182431 A CN201710182431 A CN 201710182431A CN 106894238 A CN106894238 A CN 106894238A
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- sizing agent
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/55—Epoxy resins
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention proposes a kind of silicon carbide fibre sizing agent, includes by weight：10 20 parts of main slurry, 0.5 4.5 parts of emulsifying agent, 12 parts of modification organic silicon oil, 0.5 1.5 parts of bleeding agent, 72 88 parts of deionized water.In main slurry, vinyl ester resin increased wellability and processing performance, coordinate epoxidized polybutadiene mixing rear slurry to have cohesive higher, and with good intensity, toughness, it is ensured that the intensity of fiber will not decline as the length of synnema increases.It can effectively reduce fiber lousiness and fracture of wire to the sizing agent, improve synnema intensity, effectively improve continuous carbofrax fibre performance.
Description
Technical field
The present invention relates to a kind of silicon carbide fibre sizing agent and preparation method thereof.
Background technology
Silicon carbide fibre is a kind of important tec fiber, with elevated temperature strength is big, resistant to chemical etching, wear resistance
The high, characteristic such as modulus is big, hardness is high, is widely used in the high-techs such as auto industry, space flight and aviation, rocket engine, fusion furnace
Skill field.Silicon carbide fibre has two kinds of syntheti c routes, and a kind of method is precursor pyrolysis and hot pressing, and another method is chemical vapor deposition
Area method (CVD)." polymer-derived method " is that organosilicon polymer-polymethyl silicane is made into Polycarbosilane first, then through melting
Wire drawing into precursor, then through cure treatment and high temperature sintering into silicon carbide fibre." CVD " is using fine tungsten filament or carbon
Fibril etc. makes organosilicon carry out series of chemical on high temperature heart yearn surface under nitrogen protection as carrier, and in heart yearn
Surface Creation silicon carbide fibre deposit.
At present, the mainly developed country such as Japan, U.S. of silicon carbide fiber technique comparative maturity, and technology of preparing is strict
Secrecy.Exploitation of the China to silicon carbide fibre is started late, the industrialized production of silicon carbide fibre and practical level aspect with
Western developed country all has larger gap, is mainly reflected in：(1) synnema for preparing is loose, and there is lousiness and fracture of wire
Phenomenon so that fiber is extremely difficult to continuous prodution；(2) intensity of synnema can be reduced with the increase of synnema length；(3) it is fine
The fault of construction of dimension is more, it is difficult to work out, and is unfavorable for being prepared into complex composite material.These all limit continuous carbofrax fibre
Using, but processed by appropriate starching, can effectively improve these problems, improve the intensity and practicality of fiber.
The preparation of silicon carbide fibre sizing agent is one of guardian technique in silicon carbide fibre production process, is carbonized before this
The technical formula of silica fibre sizing agent is rarely reported, and focuses primarily upon carbon fiber side for the report of inorfil sizing agent
Face.As Toray companies develop No.1-No.10 sizing agents；Countalars companies have Neoxi1971, Neoxi1969,
Neoxi1961, Neoxi18294 series sizing agent；Domestic some research institutes and unit are also ground to carbon fiber sizing agent
Make and have made some progress.Chinese Academy of Sciences's Shanxi coalification uses phase conversion emulsifying, successfully have developed and is with epoxy resin AG-80
The sizing agent of main slurry, the sizing agent improves the compatibility between carbon fiber and matrix resin, improves the interface of composite
Caking property；Cao Xia etc. adds APEO bleeding agent in polyimides and epoxy resin and is prepared for high-temperature resistance carbon fiber starching
Agent, is significantly improved through analysis shows through the carbon fiber wearability that the sizing agent is processed, and the interface of composite is cut at 350 DEG C
When shearing stress conservation rate is room temperature 75.62%；Yang Yu etc. reports a kind of modified epoxy resin sizing agent of nanosized SiO_2；
Laugh at and fine etc. have developed a kind of modified carbon fiber emulsion pasting agent of Graphene.Compared to carbon fiber, silicon carbide fibre starching difficulty
It is all higher harsher with the requirement to sizing agent, thus exploitation prepare excellent performance silicon carbide fibre sizing agent have it is important
Meaning.
The content of the invention
The present invention proposes a kind of silicon carbide fibre sizing agent, and vinyl ester resin increased wellability and processing performance, match somebody with somebody
Cyclization oxidation mixed with polybutadiene rear slurry has cohesive higher, and with good intensity, toughness, it is ensured that fiber it is strong
Degree will not decline as the length of synnema increases.It can effectively reduce fiber lousiness and fracture of wire to the sizing agent, improve synnema strong
Degree, effectively improves continuous carbofrax fibre performance.
The technical proposal of the invention is realized in this way：
A kind of silicon carbide fibre sizing agent, includes by weight：Main slurry 10-20 parts, emulsifying agent 0.5-4.5 parts, change
Property 1-2 parts of organic silicone oil, bleeding agent 0.5-1.5 parts, deionized water 72-88 parts.
Preferably, the main slurry is the mixture of vinyl ester resin and epoxidized polybutadiene, and its weight ratio is 1:1
~1:2.
Preferably, the vinyl ester resin is bisphenol type epoxy acrylic compounds vinyl ester resin.
Preferably, the emulsifying agent is aromatic nonionic emulsifying agent：NPE.
Preferably, the modification organic silicon oil is amino-modified silicone fat liquor.
Preferably, the bleeding agent is nonionic surface active agent：Sec-octyl alcohol APEO.
A kind of silicon carbide fibre sizing agent and preparation method thereof, comprises the following steps：
(1) by weight it is 1 by 10-20 parts of vinyl ester resin and epoxidized polybutadiene:1~1:2 mixing, 70
10min is stirred with 1000r/min at DEG C, it is well mixed；
(2) toward addition 0.5-4.5 parts of NPE, 1-2 parts of amino-modified silicone oil emulsion in said mixture
And 0.5-1.5 parts of sec-octyl alcohol APEO, 30min is stirred with 1000r/min at 70 DEG C, and the mixed liquor is cooled down into system
50℃；
(3) toward being slowly dropped into 72-88 parts in said mixture under being emulsified with the rotating speed cutting high of 8000r/min at 50 DEG C
Ionized water, adds water in 90min and continues to obtain uniform and stable emulsion with 1000r/min stirrings 30min after finishing, and is made after cooling
Obtain silicon carbide fibre sizing agent.
What the present invention was produced has the beneficial effect that：(1) sizing agent is emulsion-type sizing agent, and raw material is easy to get and low cost, right
It is environment-friendly.(2) by adjusting each component between proportioning, may be such that the sizing agent stability increase.(3) sizing agent can have
Effect reduces fiber lousiness and fracture of wire, improves synnema intensity, effectively improves continuous carbofrax fibre performance.
Specific 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, this
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.
Vinyl ester resin used is the V-3200 of Jinan Yi Sheng resins Co., Ltd production, technical grade.
Epoxidized polybutadiene used is the long-range development in science and technology Co., Ltd production in Wuhan, technical grade.
NPE NP-10 used is produced for Chinese medicines group Chemical Co., Ltd., is analyzed pure.
Embodiment 1
The preparation method of sizing agent is comprised the following steps in the present embodiment：
(1) by the vinyl ester resin of 10 weight portions and epoxidized polybutadiene by weight 1:1 mixing, at 70 DEG C with
1000r/min stirs 10min, is well mixed it；
(2) toward adding 0.5 weight portion NPE, 1 weight portion amino-modified silicone oil in above-mentioned (1) mixture
Emulsion and 0.5 weight portion sec-octyl alcohol APEO, 30min is stirred at 70 DEG C with 1000r/min, and the mixed liquor is cold
But 50 DEG C are made；
(3) toward being slowly dropped into 88 weight in above-mentioned (2) mixture under being emulsified with the rotating speed cutting high of 8000r/min at 50 DEG C
Part deionized water, adds water in 90min and continues to obtain uniform and stable emulsion with 1000r/min stirrings 30min after finishing, and cools down
Silicon carbide fibre sizing agent is obtained afterwards.
Embodiment 2
The preparation method of sizing agent is comprised the following steps in the present embodiment：
(1) by the vinyl ester resin of 15 weight portions and epoxidized polybutadiene by weight 1:1 mixing, at 70 DEG C with
1000r/min stirs 10min, is well mixed it；
(2) toward adding 3 weight portion NPEs, 1.5 weight portion amino-modified silicone oils in above-mentioned (1) mixture
Emulsion and 1 weight portion sec-octyl alcohol APEO, stir 30min, and the mixed liquor is cooled down at 70 DEG C with 1000r/min
50 DEG C of system；
(3) toward being slowly dropped into 79.5 weights in above-mentioned (2) mixture under being emulsified with the rotating speed cutting high of 8000r/min at 50 DEG C
Amount part deionized water, adds water in 90min and continues to obtain uniform and stable emulsion with 1000r/min stirrings 30min after finishing, cold
But silicon carbide fibre sizing agent is obtained afterwards.
Embodiment 3
The preparation method of sizing agent is comprised the following steps in the present embodiment：
(1) by the vinyl ester resin of 20 weight portions and epoxidized polybutadiene by weight 1:2 mixing, at 70 DEG C with
1000r/min stirs 10min, is well mixed it；
(2) toward adding 4.5 weight portion NPEs, 2 weight portion amino-modified silicone oils in above-mentioned (1) mixture
Emulsion and 1.5 weight portion sec-octyl alcohol APEOs, 30min is stirred at 70 DEG C with 1000r/min, and the mixed liquor is cold
But 50 DEG C are made；
(3) toward being slowly dropped into 72 weight in above-mentioned (2) mixture under being emulsified with the rotating speed cutting high of 8000r/min at 50 DEG C
Part deionized water, adds water in 90min and continues to obtain uniform and stable emulsion with 1000r/min stirrings 30min after finishing, and cools down
Silicon carbide fibre sizing agent is obtained afterwards.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (7)
1. a kind of silicon carbide fibre sizing agent, it is characterised in that include by weight：Main slurry 10-20 parts, emulsifying agent 0.5-
4.5 parts, modification organic silicon oil 1-2 parts, bleeding agent 0.5-1.5 parts, deionized water 72-88 parts.
2. a kind of silicon carbide fibre sizing agent as claimed in claim 1, it is characterised in that the main slurry is vinyl esters tree
The mixture of fat and epoxidized polybutadiene, its weight ratio is 1:1~1:2.
3. a kind of silicon carbide fibre sizing agent as claimed in claim 2, it is characterised in that the vinyl ester resin is bis-phenol
A type propylene oxide acids vinyl ester resins.
4. a kind of silicon carbide fibre sizing agent as claimed in claim 1, it is characterised in that the emulsifying agent be aromatic series it is non-from
Subtype emulsifying agent：NPE.
5. a kind of silicon carbide fibre sizing agent as claimed in claim 1, it is characterised in that the modification organic silicon oil is amino
Modified organic silicon fat liquor.
6. a kind of silicon carbide fibre sizing agent as claimed in claim 1, it is characterised in that the bleeding agent is nonionic table
Face activating agent：Sec-octyl alcohol APEO.
7. a kind of silicon carbide fibre sizing agent and preparation method thereof, it is characterised in that comprise the following steps：
(1) by weight it is 1 by 10-20 parts of vinyl ester resin and epoxidized polybutadiene:1~1:2 mixing, at 70 DEG C
10min is stirred with 1000r/min, it is well mixed；
(2) toward add in said mixture 0.5-4.5 parts of NPE, 1-2 parts of amino-modified silicone oil emulsion and
0.5-1.5 parts of sec-octyl alcohol APEO, stirs 30min, and mixed liquor cooling is made into 50 at 70 DEG C with 1000r/min
℃；
(3) toward being slowly dropped into 72-88 parts of deionization in said mixture under being emulsified with the rotating speed cutting high of 8000r/min at 50 DEG C
Water, adds water in 90min and continues to obtain uniform and stable emulsion with 1000r/min stirrings 30min after finishing, and carbon is obtained after cooling
SiClx fiber sizing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710182431.8A CN106894238A (en) | 2017-03-24 | 2017-03-24 | A kind of silicon carbide fibre sizing agent and preparation method thereof |
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| CN201710182431.8A CN106894238A (en) | 2017-03-24 | 2017-03-24 | A kind of silicon carbide fibre sizing agent and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109853238A (en) * | 2019-03-06 | 2019-06-07 | 福建立亚新材有限公司 | A kind of silicon carbide or silicon nitride fiber sizing agent and its preparation method and application |
| CN111704478A (en) * | 2020-06-12 | 2020-09-25 | 陕西元丰纺织技术研究有限公司 | Sizing method for high-strength high-modulus silicon carbide fiber |
| 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 yarn stuck with sizing agent |
| CN101858037A (en) * | 2010-06-18 | 2010-10-13 | 济南大学 | Emulsion type carbon fiber sizing agent and preparation method and application thereof |
| CN103132327A (en) * | 2013-03-18 | 2013-06-05 | 中国人民解放军国防科学技术大学 | Sizing agent applied to constant SiC (Silicon Carbide) fiber and preparation method and application thereof |
-
2017
- 2017-03-24 CN CN201710182431.8A patent/CN106894238A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07166475A (en) * | 1993-12-14 | 1995-06-27 | Sumitomo Chem Co Ltd | Alumina yarn stuck with sizing agent |
| CN101858037A (en) * | 2010-06-18 | 2010-10-13 | 济南大学 | Emulsion type carbon fiber sizing agent and preparation method and application thereof |
| CN103132327A (en) * | 2013-03-18 | 2013-06-05 | 中国人民解放军国防科学技术大学 | Sizing agent applied to constant SiC (Silicon Carbide) fiber and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 唐磊等: "《轻量化材料技术》", 31 January 2014, 国防工业出版社 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109853238A (en) * | 2019-03-06 | 2019-06-07 | 福建立亚新材有限公司 | A kind of silicon carbide or silicon nitride fiber sizing agent and its preparation method and application |
| CN111704478A (en) * | 2020-06-12 | 2020-09-25 | 陕西元丰纺织技术研究有限公司 | Sizing method for high-strength high-modulus silicon carbide fiber |
| 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 special sizing agent for nitride fibers |
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