CN110054858A - A kind of silane-modified silicon carbide fibre and preparation method thereof - Google Patents
A kind of silane-modified silicon carbide fibre and preparation method thereof Download PDFInfo
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- CN110054858A CN110054858A CN201910214157.7A CN201910214157A CN110054858A CN 110054858 A CN110054858 A CN 110054858A CN 201910214157 A CN201910214157 A CN 201910214157A CN 110054858 A CN110054858 A CN 110054858A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
- C08L33/12—Homopolymers or copolymers of methyl methacrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of silane-modified silicon carbide fibres, each raw material including following weight parts: silicon carbide fibre 120-140, silane coupling agent kh550 1-3,2,2- dihydromethyl propionic acid 2-4, ethyl orthosilicate 30-40, polyamide wax micropowder 3-5, epoxy prapanol 1-2, barium stearate 2-3, methyl methacrylate 16-20, catalyst 0.07-0.1, polytetrafluoroethylene (PTFE) 5-8, triethylamine 0.8-1, the finished composite material that the present invention obtains not only has good intensity and toughness, and mechanical stability is good, comprehensive performance is superior.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of silane-modified silicon carbide fibre and preparation method thereof.
Background technique
Silicon carbide fibre is made through spinning, carbonization or vapor deposition with β-carbonization using organo-silicon compound as raw material
The inorfil of silicon structure, belongs to ceramic fibre class, and the maximum operation (service) temperature of silicon carbide fibre is up to 1200 DEG C, heat resistance and oxytolerant
The property changed is superior to carbon fiber, and intensity is up to 1960~4410MPa, and strength retention is 80% or more under maximum operation (service) temperature, mould
Amount is 176.4~294GPa, and chemical stability might as well.
Silicon carbide fibre is mainly used as heat-resisting material and reinforcing material, and heat-resisting material includes heatshield material, resistance to height
Warm conveyer belt, filtering high temperature gas or filter cloth of molten metal etc..When being used as reinforcing material, often closed with carbon fiber or glass fibre
With, with enhance metal (such as aluminium) and ceramics based on, be such as made into the brake block, engine blade, landing gear case of jet plane
With airframe material etc., sports goods can be used as, chopped strand then can be used as high temperature furnace material etc..
However currently, the composite material stability prepared using silicon carbide fibre as raw material is lower, therefore, how to improve compound
The stability of material is the emphasis studied at present.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of silane-modified silicon carbide fibre and its preparation sides
Method.
To achieve the above object, the present invention uses following technical scheme.
A kind of silane-modified silicon carbide fibre, each raw material including following weight parts:
Silicon carbide fibre 120-140, silane coupling agent kh550 1-3,2,2- dihydromethyl propionic acid 2-4, ethyl orthosilicate 30-
40, polyamide wax micropowder 3-5, epoxy prapanol 1-2, barium stearate 2-3, methyl methacrylate 16-20, catalyst 0.07-
0.1, polytetrafluoroethylene (PTFE) 5-8, triethylamine 0.8-1.
Further, the catalyst is lithium methoxide.
A kind of preparation method of silane-modified silicon carbide fibre, comprising the following steps:
(1) silane coupling agent kh550 is taken, is added in the dehydrated alcohol of 13-20 times of its weight, increasing temperature is 50-55 DEG C, is added
Enter silicon carbide fibre, insulated and stirred 1-2 hours, ethyl alcohol is distilled off, obtains amino silane modified polymer；
(2) 2,2- dihydromethyl propionic acid, ethyl orthosilicate mixing are taken, is added in the deionized water of 36-40 times of mixture weight,
It is stirred to react 3-5 hours, obtains sol solution；
(3) above-mentioned amino silane modified polymer is taken, is added in sol solution, increasing temperature is 70-75 DEG C, insulated and stirred 1-
It 2 hours, filters, filter cake is washed, is sent in sintering furnace, it is 3-4 hours dry at 170-200 DEG C, it is cooled to room temperature, obtains fine
Tie up colloidal sol；
(4) polyamide wax micropowder, barium stearate mixing are taken, is added in the toluene of 6-8 times of mixture weight, stirs evenly, obtain
Toluene solution；
(5) methyl methacrylate, polytetrafluoroethylene (PTFE), epoxy prapanol mixing are taken, is sent in stainless steel cauldron, is passed through nitrogen
Gas, adjusting temperature of reaction kettle is 95-105 DEG C, is stirred to react 1-2 hours, and catalyst is added, and adjusting temperature of reaction kettle is 150-
160 DEG C, insulated and stirred 2-3 hours, discharging cooling obtained epoxy-modified polymer；
(6) Fibersol-2 is taken, is added in above-mentioned toluene solution, stirs evenly, with above-mentioned epoxy-modified mixed with polymers, stirring
Uniformly, triethylamine is added, is sent in reaction kettle, insulated and stirred 100-130 minutes at 150-160 DEG C, discharging cooling is done
It is dry to get the silane-modified silicon carbide fibre.
Further, drying temperature described in step (6) is 80-90 DEG C.
The invention has the benefit that the present invention uses silane coupling agent kh550 to handle silicon carbide fibre first, amino is obtained
Silane modified polymer, then with 2,2- dihydromethyl propionic acid for presoma, with 2,2- dihydromethyl propionic acid for promotor, will obtain
Colloidal sol be blended with amino silane modified polymer, realize the effective compatible of colloidal sol and fiber, obtain Fibersol-2, use ring later
Oxygen propyl alcohol handles polytetrafluoroethylene (PTFE), by obtained epoxides and Fibersol-2 blending reaction, promotion epoxy cross-linking, obtain at
Product composite material not only has good intensity and toughness, and mechanical stability is good, and comprehensive performance is superior.
Specific embodiment
As described below is the embodiment of the present invention 1.
A kind of silane-modified silicon carbide fibre, each raw material including following weight parts:
Silicon carbide fibre 120, silane coupling agent kh550 1,2,2- dihydromethyl propionic acid 2, ethyl orthosilicate 30, polyamide wax are micro-
Powder 3, epoxy prapanol 1, barium stearate 2, methyl methacrylate 16, catalyst 0.07, polytetrafluoroethylene (PTFE) 5, triethylamine 0.8.
The catalyst is lithium methoxide.
A kind of preparation method of silane-modified silicon carbide fibre, comprising the following steps:
(1) silane coupling agent kh550 is taken, is added in the dehydrated alcohol of 13 times of its weight, increasing temperature is 50 DEG C, and carbonization is added
Silica fibre insulated and stirred 1 hour, is distilled off ethyl alcohol, obtains amino silane modified polymer；
(2) 2,2- dihydromethyl propionic acid, ethyl orthosilicate mixing are taken, is added in 36 times of mixture weight of deionized water, stirs
Reaction 3 hours is mixed, sol solution is obtained；
(3) above-mentioned amino silane modified polymer is taken, is added in sol solution, increasing temperature is 70 DEG C, and insulated and stirred 1 is small
When, it filters, filter cake is washed, is sent in sintering furnace, it is 3 hours dry at 170 DEG C, it is cooled to room temperature, obtains Fibersol-2；
(4) polyamide wax micropowder, barium stearate mixing are taken, is added in 6 times of mixture weight of toluene, is stirred evenly, obtain first
Benzole soln；
(5) methyl methacrylate, polytetrafluoroethylene (PTFE), epoxy prapanol mixing are taken, is sent in stainless steel cauldron, is passed through nitrogen
Gas, adjusting temperature of reaction kettle is 95 DEG C, is stirred to react 1 hour, and catalyst is added, and adjusting temperature of reaction kettle is 150 DEG C, and heat preservation is stirred
It mixes 2 hours, discharging cooling obtains epoxy-modified polymer；
(6) Fibersol-2 is taken, is added in above-mentioned toluene solution, stirs evenly, with above-mentioned epoxy-modified mixed with polymers, stirring
Uniformly, triethylamine is added, is sent in reaction kettle, insulated and stirred 100 minutes at 150 DEG C, discharging cooling is dry to get institute
State silane-modified silicon carbide fibre.
Drying temperature described in step (6) is 80 DEG C.
As described below is the embodiment of the present invention 2.
A kind of silane-modified silicon carbide fibre, each raw material including following weight parts:
Silicon carbide fibre 140, silane coupling agent kh550 3,2,2- dihydromethyl propionic acid 4, ethyl orthosilicate 40, polyamide wax are micro-
Powder 5, epoxy prapanol 2, barium stearate 3, methyl methacrylate 20, catalyst 0.1, polytetrafluoroethylene (PTFE) 8, triethylamine 1.
The catalyst is lithium methoxide.
A kind of preparation method of silane-modified silicon carbide fibre, comprising the following steps:
(1) silane coupling agent kh550 is taken, is added in the dehydrated alcohol of 20 times of its weight, increasing temperature is 55 DEG C, and carbonization is added
Silica fibre insulated and stirred 2 hours, is distilled off ethyl alcohol, obtains amino silane modified polymer；
(2) 2,2- dihydromethyl propionic acid, ethyl orthosilicate mixing are taken, is added in 40 times of mixture weight of deionized water, stirs
Reaction 5 hours is mixed, sol solution is obtained；
(3) above-mentioned amino silane modified polymer is taken, is added in sol solution, increasing temperature is 75 DEG C, and insulated and stirred 2 is small
When, it filters, filter cake is washed, is sent in sintering furnace, it is 4 hours dry at 200 DEG C, it is cooled to room temperature, obtains Fibersol-2；
(4) polyamide wax micropowder, barium stearate mixing are taken, is added in 8 times of mixture weight of toluene, is stirred evenly, obtain first
Benzole soln；
(5) methyl methacrylate, polytetrafluoroethylene (PTFE), epoxy prapanol mixing are taken, is sent in stainless steel cauldron, is passed through nitrogen
Gas, adjusting temperature of reaction kettle is 105 DEG C, is stirred to react 2 hours, and catalyst is added, and adjusting temperature of reaction kettle is 160 DEG C, heat preservation
Stirring 3 hours, discharging cooling, obtains epoxy-modified polymer；
(6) Fibersol-2 is taken, is added in above-mentioned toluene solution, stirs evenly, with above-mentioned epoxy-modified mixed with polymers, stirring
Uniformly, triethylamine is added, is sent in reaction kettle, insulated and stirred 130 minutes at 160 DEG C, discharging cooling is dry to get institute
State silane-modified silicon carbide fibre.
Drying temperature described in step (6) is 90 DEG C.
Performance test:
The silane-modified silicon carbide fibre of the embodiment of the present invention 1:
Bending strength: 391Mpa；
Tensile strength: 278Mpa；
Fracture toughness: 27.5MPam1/2；
The silane-modified silicon carbide fibre of the embodiment of the present invention 2:
Bending strength: 372Mpa；
Tensile strength: 255Mpa；
Fracture toughness: 24.0MPam1/2。
Claims (4)
1. a kind of silane-modified silicon carbide fibre, which is characterized in that each raw material including following weight parts:
Silicon carbide fibre 120-140, silane coupling agent kh550 1-3,2,2- dihydromethyl propionic acid 2-4, ethyl orthosilicate 30-
40, polyamide wax micropowder 3-5, epoxy prapanol 1-2, barium stearate 2-3, methyl methacrylate 16-20, catalyst 0.07-
0.1, polytetrafluoroethylene (PTFE) 5-8, triethylamine 0.8-1.
2. a kind of silane-modified silicon carbide fibre according to claim 1, which is characterized in that the catalyst is methanol
Lithium.
3. a kind of preparation method of silane-modified silicon carbide fibre as described in claim 1, which is characterized in that including following step
It is rapid:
(1) silane coupling agent kh550 is taken, is added in the dehydrated alcohol of 13-20 times of its weight, increasing temperature is 50-55 DEG C, is added
Enter silicon carbide fibre, insulated and stirred 1-2 hours, ethyl alcohol is distilled off, obtains amino silane modified polymer；
(2) 2,2- dihydromethyl propionic acid, ethyl orthosilicate mixing are taken, is added in the deionized water of 36-40 times of mixture weight,
It is stirred to react 3-5 hours, obtains sol solution；
(3) above-mentioned amino silane modified polymer is taken, is added in sol solution, increasing temperature is 70-75 DEG C, insulated and stirred 1-
It 2 hours, filters, filter cake is washed, is sent in sintering furnace, it is 3-4 hours dry at 170-200 DEG C, it is cooled to room temperature, obtains fine
Tie up colloidal sol；
(4) polyamide wax micropowder, barium stearate mixing are taken, is added in the toluene of 6-8 times of mixture weight, stirs evenly, obtain
Toluene solution；
(5) methyl methacrylate, polytetrafluoroethylene (PTFE), epoxy prapanol mixing are taken, is sent in stainless steel cauldron, is passed through nitrogen
Gas, adjusting temperature of reaction kettle is 95-105 DEG C, is stirred to react 1-2 hours, and catalyst is added, and adjusting temperature of reaction kettle is 150-
160 DEG C, insulated and stirred 2-3 hours, discharging cooling obtained epoxy-modified polymer；
(6) Fibersol-2 is taken, is added in above-mentioned toluene solution, stirs evenly, with above-mentioned epoxy-modified mixed with polymers, stirring
Uniformly, triethylamine is added, is sent in reaction kettle, insulated and stirred 100-130 minutes at 150-160 DEG C, discharging cooling is done
It is dry to get the silane-modified silicon carbide fibre.
4. a kind of silane-modified silicon carbide fibre according to claim 3, which is characterized in that done described in step (6)
Dry temperature is 80-90 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910214157.7A CN110054858A (en) | 2019-03-20 | 2019-03-20 | A kind of silane-modified silicon carbide fibre and preparation method thereof |
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| CN201910214157.7A CN110054858A (en) | 2019-03-20 | 2019-03-20 | A kind of silane-modified silicon carbide fibre and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113716868A (en) * | 2021-09-28 | 2021-11-30 | 佛山市帆思科材料技术有限公司 | High-temperature matte type digital ink-jet printing glaze |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113716868A (en) * | 2021-09-28 | 2021-11-30 | 佛山市帆思科材料技术有限公司 | High-temperature matte type digital ink-jet printing glaze |
| CN113716868B (en) * | 2021-09-28 | 2022-08-02 | 佛山市帆思科材料技术有限公司 | High-temperature matte type digital ink-jet printing glaze |
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Application publication date: 20190726 |