CN105670321B - A kind of heat-insulated cork composite material of impact resistance and preparation method thereof - Google Patents
A kind of heat-insulated cork composite material of impact resistance and preparation method thereof Download PDFInfo
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- CN105670321B CN105670321B CN201610202065.3A CN201610202065A CN105670321B CN 105670321 B CN105670321 B CN 105670321B CN 201610202065 A CN201610202065 A CN 201610202065A CN 105670321 B CN105670321 B CN 105670321B
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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
- C08L97/00—Compositions of lignin-containing materials
- C08L97/007—Cork
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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Abstract
The present invention relates to heat-insulated cork composite material of a kind of impact resistance and preparation method thereof, pass through the synergistic effect of modified phenolic adhesive, phenyl siloxane rubber and organic fiber in cork composite material, the problem of existing cork is heat-resisting and toughness is poor is overcome, cork composite material is had excellent resistance to ablation and impact resistance concurrently.Cork composite material preparation method technique provided by the invention is simple and is easy to regulate and control, and cost is low, there is commercial introduction application value.
Description
Technical field
The present invention relates to heat-insulated cork composite material of a kind of impact resistance and preparation method thereof, belongs to composite material and prepares neck
Domain.
Background technology
Cork has preferable heat-proof quality, and civil field, such as thermos cork are widely used in as heat-barrier material, is used for
Soft thin plate of heating furnace, heater and heat-insulating etc..Cork has that thermal conductivity factor is low, light specific gravity, processing performance are good, source
Extensively, the advantages that cheap, also applied in the thermal protection field of all kinds of aerospace vehicles.Such as " the arctic in the U.S.
Star ", " people's militia " guided missile are used as heat-insulated cone, Apollo Personnel investigation Program by the use of cork " airship employs vegetable cork as heat shield, " Arian "
Cork sheet is posted on carrier rocket satellite fairing and three grade low-temp storage tanks.The CZ-3 in China, CZ-2E carrier rocket satellite are whole
Shell, booster rocket radome fairing shell are also covered with vegetable cork between stream cover, two three-level levels.
Domestic heat-insulated cork composite material is 301 (trade mark) vegetable corks at present, but 301 vegetable cork thermal conductivities are higher than
External similar trade mark P50 corks (301 cork thermal conductivity 0.10W/mK, P50 cork thermal conductivity 0.08W/mK), and resistance to punching
Hit poor-performing (301 cork impact strength 1.4kJ/m2, P50 cork impact strengths 2.5kJ/m2), easily it is subject at some
The position of impact force is particularly easy to breakage occur, the thermal protective performance of product is influenced, in addition, the cork flexibility that impact resistance is low
It is poor, the stickup of cork layer is carried out in the larger section of some tapers, cork bending is applied easily to be cracked on the surface of section,
Largely effect on the mechanical property and thermal protective performance of cork layer.The above-mentioned deficiency of existing cork, is allowed to answering in high-tech sector
With limited.
The content of the invention
The object of the present invention is to provide heat-insulated cork composite material of a kind of impact resistance and preparation method thereof, by being mixed in cork
Close and phenolic resin, phenyl siloxane rubber and organic fiber are added in material to realize the raising of composite material impact resistance and heat-proof quality.
The cork composite material of the present invention, is made of following weight parts proportioning：Cork particle 80~100, phenolic resin glue
Stick 5~20, phenyl siloxane rubber 2~15, organic fiber 0.5~5.It is preferred that cork particle 90~100, synvaren 10
~20, phenyl siloxane rubber 4~12, organic fiber 1~4, the impact resistance of cork composite material, heat-proof quality are high under the proportioning.
The synvaren is one in boron modified phenolic resin, ba phenolic resin or magnesium synvaren
Kind or several mixtures, heat resistance is improved using synvaren.
The phenyl siloxane rubber is one or both of methyl phenyl silicone rubber or methyl phenyl vinyl silicone rubber, excellent
Select methyl phenyl silicone rubber.In preparation process, methyl phenyl silicone rubber craftsmanship is more preferable.
The phenyl molar content scope of the phenyl siloxane rubber is 5~40%, preferably phenyl molar content scope for 5~
30%, in the range of the phenyl content methyl phenyl silicone rubber be easily mixed, good manufacturability.
The organic fiber is Fanglun 1313, polyphenylsulfone nylon, gathers to benzimidazole fibre
Dimension, polyhenylene pyrido diimidazole fiber, gather to penylene benzo-dioxazole fiber, polyphenylene sulfide fibre, polyether ketone fiber, polyethers
One or more of mixtures in ether ketone fiber, polypyrrole fiber.Above-mentioned organic fiber good toughness, intensity are high, high temperature resistant, right
The impact resistance of cork composite material plays a key effect.
The length range of the organic fiber is 5~30mm, and preferred length scope is 5~10mm.In the length range
Fiber is chopped strand, and good dispersion, is not easy to reunite.
A kind of preparation method of the heat-insulated cork composite material of impact resistance, specific preparation process and condition are as follows：
(1) cork powder particle is sieved, filters out the cork particle that particle diameter is 30~60 mesh；
(2) cork powder after screening is heat-treated, heat treatment time is 5~30h, the cork after being heat-treated
Powder；
(3) pretreated cork particle, modified phenolic adhesive, phenyl siloxane rubber, organic fiber mechanical agitation are mixed equal
It is even, obtain mixed material；Cork particle 80~100, synvaren 5~20, phenyl siloxane rubber 2~15, organic fiber
0.5~5；
(4) mixed material is put into mould, applies 1~10 ton of pressure, mould, which is placed in vulcanizer heating plate, to be consolidated
Change, solidification temperature is 100~200 DEG C, and hardening time is 1~12h；
(5) mould is taken out after curing, is cooled to room temperature, die sinking sampling obtains cork composite material.
Heat treatment described in step (2) is 100~150 DEG C of normal pressure drying, vacuum drying or high temperature steam treatments.
Curing described in step (4) cures for isothermal curing or gradient increased temperature.
Heat treatment described in step b) is normal pressure drying, vacuum drying or high temperature steam treatment；
Curing described in step d) can be that isothermal curing or gradient increased temperature cure, and wherein gradient increased temperature cures favourable
In the shaping of special-shaped structure piece, curing can be made more abundant, performance higher.
The present invention compared with prior art the advantages of be：Cork composite material prepared by the present invention, density is low, maintains
Good mechanical property.And by the synergistic effect of modified phenolic adhesive, phenyl siloxane rubber and organic fiber, overcome existing soft
The problem of heat-resisting and toughness of wood is poor, makes cork composite material have excellent thermal insulation and impact resistance (cork of the invention concurrently
Thermal conductivity scope at 150 DEG C of composite material is 0.05~0.08W/mK, and impact strength scope is 2.2~4.0kJ/m2；
And the thermal conductivity scope at existing 150 DEG C of 301 trade mark cork composite material is 0.09~0.12W/mK, impact strength scope
For 0.6~1.0kJ/m2).Cork composite material preparation method technique provided by the invention is simple and is easy to regulate and control, without special
Process equipment, cost is low, there is commercial introduction application value.
Embodiment
With reference to embodiment, the present invention is further described, but does not form limiting the scope of the invention.
Embodiment 1
(1) using natural cork powder as raw material, the granulated cork that particle diameter is 30~60 mesh is filtered out；
(2) the above-mentioned granulated cork of 200g is weighed, the normal pressure at 120 DEG C is laid in container and dries, taken out after 24h；
(3) by the granulated cork after normal pressure drying and processing, boron modification modified phenolic adhesive, (phenyl rubs methyl phenyl silicone rubber
Your content is 20%) to press proportion by weight 100：15：5 carry out mechanical agitation mixing, and incorporation time 30min, continuously adds matter
Measure the Fanglun 1313 (5~10mm of length) that part is 2 and mix 30min, obtain mixed material；
(4) said mixture material being put into mould, applies 5 tons of pressure, mould, which is placed on vulcanizer, carries out isothermal curing,
Solidification temperature is 160 DEG C, hardening time 10h；
(5) mould is taken out after curing, is cooled to room temperature, die sinking sampling obtains cork composite material.
Obtained cork composite material is tested, 150 DEG C of thermal conductivities are 0.08W/mK, and impact strength is
2.5kJ/m2。
Embodiment 2
(1) using natural cork powder as raw material, the granulated cork that particle diameter is 30~60 mesh is filtered out；
(2) the above-mentioned granulated cork of 200g is weighed, the normal pressure at 100 DEG C is laid in container and dries, taken out after 24h；
(3) by the granulated cork after normal pressure drying and processing, boron modification modified phenolic adhesive, (phenyl rubs methyl phenyl silicone rubber
Your content is 10%) to press proportion by weight 100：14：8 carry out mechanical agitation mixing, and incorporation time 50min, continuously adds matter
Amount part mixes 60min for 1.8 gather to benzimidazole fiber (5~10mm of length), obtains mixed material；
(4) said mixture material is put into mould, applies 10 tons of pressure, mould is placed on progress constant temperature on vulcanizer and consolidates
Change, solidification temperature is 180 DEG C, hardening time 6h；
(5) mould is taken out after curing, is cooled to room temperature, die sinking sampling obtains cork composite material.
Obtained cork composite material is tested, 150 DEG C of thermal conductivities are 0.08W/mK, and impact strength is
2.2kJ/m2。
Embodiment 3
(1) using natural cork powder as raw material, the granulated cork that particle diameter is 30~60 mesh is filtered out；
(2) the above-mentioned granulated cork of 200g is weighed, the vacuum drying at 100 DEG C is laid in container, is taken out after 12h；
(3) granulated cork, boron modification modified phenolic adhesive, methyl phenyl vinyl silicone rubber after vacuum drying is handled
(phenyl molar content is 15%) presses proportion by weight 80：12：5 carry out mechanical agitation mixing, and incorporation time 30min, continues
Add the polyhenylene pyrido diimidazole fiber (5~10mm of length) that mass parts are 2 and mix 40min, obtain mixed material；
(4) said mixture material is put into mould, applies 5 tons of pressure, mould, which is placed on vulcanizer, carries out gradient increased temperature
Cure, the first stage：Cure 6h, second stage at 120 DEG C：Cure 4h at 180 DEG C；
(5) mould is taken out after curing, is cooled to room temperature, die sinking sampling obtains cork composite material.
Obtained cork composite material is tested, 150 DEG C of thermal conductivities are 0.07W/mK, and impact strength is
2.8kJ/m2。
Embodiment 4
(1) using natural cork powder as raw material, the granulated cork that particle diameter is 30~60 mesh is filtered out；
(2) the above-mentioned granulated cork of 200g is weighed, the vacuum drying at 120 DEG C is laid in container, is taken out after 8h；
(3) granulated cork, boron modification modified phenolic adhesive after vacuum drying is handled, (phenyl rubs methyl phenyl silicone rubber
Your content is 5%) to press proportion by weight 90：13：9 carry out mechanical agitation mixing, and incorporation time 30min, continuously adds quality
Part mixes 60min for 2.2 polyetheretherketonefiber fiber (5~10mm of length), obtains mixed material；
(4) said mixture material is put into mould, applies 8 tons of pressure, mould, which is placed on vulcanizer, carries out gradient increased temperature
Cure, the first stage：Cure 4h, second stage at 150 DEG C：Cure 4h at 180 DEG C；
(5) mould is taken out after curing, is cooled to room temperature, die sinking sampling obtains cork composite material.
Obtained cork composite material is tested, 150 DEG C of thermal conductivities are 0.08W/mK, and impact strength is
3.0kJ/m2。
Embodiment 5
(1) using natural cork powder as raw material, the granulated cork that particle diameter is 30~60 mesh is filtered out；
(2) the above-mentioned granulated cork of 200g is weighed, the normal pressure at 120 DEG C is laid in container and dries, taken out after 24h；
(3) by the granulated cork after normal pressure drying and processing, boron modification modified phenolic adhesive, (phenyl rubs methyl phenyl silicone rubber
Your content is 30%) to press proportion by weight 100：16：6 carry out mechanical agitation mixing, and incorporation time 45min, continuously adds matter
Measure the Fanglun 1313 (5~10mm of length) that part is 2.0 and mix 60min, obtain mixed material；
(4) said mixture material is put into mould, applies 10 tons of pressure, mould, which is placed on vulcanizer, carries out gradient increased temperature
Cure, the first stage：Cure 3h, second stage at 120 DEG C：Cure 3h, phase III at 150 DEG C：Cure 2h at 180 DEG C；；
(5) mould is taken out after curing, is cooled to room temperature, die sinking sampling obtains cork composite material.
Obtained cork composite material is tested, 150 DEG C of thermal conductivities are 0.07W/mK, and impact strength is
3.4kJ/m2。
Embodiment 6
(1) using natural cork powder as raw material, the granulated cork that particle diameter is 30~60 mesh is filtered out；
(2) the above-mentioned granulated cork of 200g is weighed, the normal pressure at 120 DEG C is laid in container and dries, taken out after 24h；
(3) by the granulated cork after normal pressure drying and processing, boron modification modified phenolic adhesive, methyl phenyl vinyl silicone rubber
(phenyl molar content is 5%) presses proportion by weight 100：10：10 carry out mechanical agitation mixing, and incorporation time 60min, continues
Add the polyphenylene sulfide fibre (5~10mm of length) that mass parts are 3.5 and mix 60min, obtain mixed material；
(4) said mixture material is put into mould, applies 10 tons of pressure, mould, which is placed on vulcanizer, carries out gradient increased temperature
Cure, the first stage：Cure 4h, second stage at 120 DEG C：Cure 5h at 150 DEG C；
(5) mould is taken out after curing, is cooled to room temperature, die sinking sampling obtains cork composite material.
Obtained cork composite material is tested, 150 DEG C of thermal conductivities are 0.08W/mK, and impact strength is
3.6kJ/m2。
Embodiment 7
(1) using natural cork powder as raw material, the granulated cork that particle diameter is 30~60 mesh is filtered out；
(2) the above-mentioned granulated cork of 200g is weighed, the normal pressure at 150 DEG C is laid in container and dries, taken out after 5h；
(3) by the granulated cork after normal pressure drying and processing, boron modification modified phenolic adhesive, (phenyl rubs methyl phenyl silicone rubber
Your content is 20%) to press proportion by weight 100：18：11 carry out mechanical agitation mixing, and incorporation time 90min, continuously adds matter
Measure the Fanglun 1313 (5~10mm of length) that part is 1.5 and mix 60min, obtain mixed material；
(4) said mixture material being put into mould, applies 5 tons of pressure, mould, which is placed on vulcanizer, carries out isothermal curing,
Solidification temperature is 180 DEG C, hardening time 12h；
(5) mould is taken out after curing, is cooled to room temperature, die sinking sampling obtains cork composite material.
Obtained cork composite material is tested, 150 DEG C of thermal conductivities are 0.05W/mK, and impact strength is
3.5kJ/m2。
Embodiment 8
(1) using natural cork powder as raw material, the granulated cork that particle diameter is 30~60 mesh is filtered out；
(2) the above-mentioned granulated cork of 200g is weighed, the normal pressure at 100 DEG C is laid in container and dries, taken out after 30h；
(3) by the granulated cork after normal pressure drying and processing, boron modification modified phenolic adhesive, (phenyl rubs methyl phenyl silicone rubber
Your content is 24%) to press proportion by weight 100：10：12 carry out mechanical agitation mixing, and incorporation time 90min, continuously adds matter
Measure the polyetheretherketonefiber fiber (5~10mm of length) that part is 3.8 and mix 60min, obtain mixed material；
(4) said mixture material is put into mould, applies 10 tons of pressure, mould, which is placed on vulcanizer, carries out gradient increased temperature
Cure, the first stage：Cure 2h, second stage at 120 DEG C：Cure 3h, phase III at 150 DEG C：Cure 4h at 180 DEG C；；
(5) mould is taken out after curing, is cooled to room temperature, die sinking sampling obtains cork composite material.
Obtained cork composite material is tested, 150 DEG C of thermal conductivities are 0.06W/mK, and impact strength is
4.0kJ/m2。
Claims (10)
- A kind of 1. heat-insulated cork composite material of impact resistance, it is characterised in that：Its weight forms：Cork particle 80~100, synvaren 5~20, phenyl siloxane rubber 2~15, organic fiber 0.5~5.
- A kind of 2. heat-insulated cork composite material of impact resistance according to claim 1, it is characterised in that：The cork particle 90 ~100, synvaren 10~20, phenyl siloxane rubber 4~12, organic fiber 1~4.
- A kind of 3. heat-insulated cork composite material of impact resistance according to claim 1 or 2, it is characterised in that：The phenolic aldehyde tree Fat adhesive is one or more of mixtures in boron modified phenolic resin, ba phenolic resin or magnesium synvaren.
- A kind of 4. heat-insulated cork composite material of impact resistance according to claim 1 or 2, it is characterised in that：The phenyl silicon Rubber is one or both of methyl phenyl silicone rubber or methyl phenyl vinyl silicone rubber.
- A kind of 5. heat-insulated cork composite material of impact resistance according to claim 1 or 2, it is characterised in that：The phenyl silicon The phenyl molar content scope of rubber is 5~40%.
- A kind of 6. heat-insulated cork composite material of impact resistance according to claim 1, it is characterised in that：The organic fiber is Fanglun 1313, polyphenylsulfone nylon, gather to benzimidazole fiber, polyhenylene pyrido diimidazole fibre Dimension, gather in penylene benzo-dioxazole fiber, polyphenylene sulfide fibre, polyether ketone fiber, polyetheretherketonefiber fiber, polypyrrole fiber One or more of mixtures.
- A kind of 7. heat-insulated cork composite material of impact resistance according to claim 1 or 6, it is characterised in that：Organic fibre The length range of dimension is 5~30mm.
- A kind of 8. preparation method of the heat-insulated cork composite material of impact resistance, it is characterised in that：Specific preparation process and condition are as follows：(1) cork powder particle is sieved, filters out the cork particle that particle diameter is 30~60 mesh；(2) cork powder after screening is heat-treated, heat treatment time is 5~30h, the cork powder after being heat-treated；(3) pretreated cork particle, modified phenolic adhesive, phenyl siloxane rubber, organic fiber mechanical agitation are uniformly mixed, obtained To mixed material；Cork particle 80~100, synvaren 5~20, phenyl siloxane rubber 2~15, organic fiber 0.5~ 5；(4) mixed material being put into mould, applies 1~10 ton of pressure, mould, which is placed in vulcanizer heating plate, to be cured, Gu It is 100~200 DEG C to change temperature, and hardening time is 1~12h；(5) mould is taken out after curing, is cooled to room temperature, die sinking sampling obtains cork composite material.
- 9. the preparation method of cork composite material according to claim 8, it is characterised in that：Heat described in step (2) Handle as 100~150 DEG C of normal pressure drying, vacuum drying or high temperature steam treatments.
- 10. the preparation method of cork composite material according to claim 8, it is characterised in that：Consolidating described in step (4) Change method cures for isothermal curing or gradient increased temperature.
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| CN108017875A (en) * | 2017-12-08 | 2018-05-11 | 浙江工业大学之江学院 | A kind of electroplating tooling thermostabilization fabroil and its manufacture method |
| CN108437305A (en) * | 2018-04-10 | 2018-08-24 | 中国科学院长春应用化学研究所 | A kind of moulding process of high-performance thermal protection cork heterotypic material |
| CN110396365B (en) * | 2019-06-27 | 2021-08-10 | 航天材料及工艺研究所 | Flexible protective layer, cork composite material structure with flexible protective layer and preparation method of cork composite material structure |
| CN113700710B (en) * | 2021-08-25 | 2023-04-18 | 湖北三江航天红阳机电有限公司 | Method for sticking cork wood |
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| CN101558120A (en) * | 2006-11-13 | 2009-10-14 | M·马纳格门特-特克斯有限公司 | Synthetic cork compound |
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| CN101558120A (en) * | 2006-11-13 | 2009-10-14 | M·马纳格门特-特克斯有限公司 | Synthetic cork compound |
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| 软木复合材料研究现状与发展趋势;宋孝周等;《西北林学院学报》;20111231;第26卷(第4期);第210-213页 * |
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