CN105670321A - Impact-resistant heat-insulation cork composite material and preparation method thereof - Google Patents
Impact-resistant heat-insulation cork composite material and preparation method thereof Download PDFInfo
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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
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- 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 invention relates to an impact-resistant heat-insulation cork composite material and a preparation method thereof. Under the synergistic actions of a phenolic adhesive, a phenyl silicon rubber and organic fibers in the cork composite material, the cork composite material solves the problems of poor heat resistance and poor toughness, and thus, has excellent ablation resistance and impact resistance. The preparation method of the cork composite material is simple in technique and easy to control, is low in cost, and has industrial popularization and application meanings.
Description
Technical field
The present invention relates to a kind of shock-resistant heat insulation cork composite material and preparation method thereof, belong to field of composite material preparation.
Background technology
Cork has good heat-proof quality, is widely used in civil area as heat-barrier material, such as thermos cork, for soft the thin plate etc. of heating furnace, heater and heat-insulating. Cork has that heat conductivity is low, light specific gravity, processing performance are good, wide material sources, the advantage such as cheap, have also been obtained application in the thermal protection field of all kinds of aerospace vehicles. " Polaris ", " people's militia " guided missile cork of the such as U.S. is as heat insulation cone, Apollo Personnel investigation Program " airship have employed vegetable cork as heat shield, " Arian " carrier rocket satellite fairing and all post cork sheet on three grade low-temp storage tanks. CZ-3, the CZ-2E carrier rocket satellite fairing of China, two or three grades of inter-stage shells, booster rocket trousers shells are also covered with vegetable cork.
Current domestic heat insulation cork composite material is 301 (trade mark) vegetable cork, but 301 vegetable cork thermal conductivities are higher than external similar trade mark P50 cork (301 cork thermal conductivity 0.10W/m K, P50 cork thermal conductivity 0.08W/m K), and poor (the 301 cork impact strength 1.4kJ/m of impact resistance2, P50 cork impact strength 2.5kJ/m2), it is easily subject to the especially easy appearance breakage in position of impulsive force at some, affect the thermal protective performance of product, additionally, the cork flexibility that impact resistance is low is poor, carry out the stickup of cork layer in the section that some taperings are bigger, cork bending is applied and is easily cracked on the surface of section, largely effects on mechanical property and the thermal protective performance of cork layer. The above-mentioned deficiency of existing cork, so as to the application in high-tech sector is limited.
Summary of the invention
It is an object of the invention to provide a kind of shock-resistant heat insulation cork composite material and preparation method thereof, realize that composite is shock-resistant and the raising of heat-proof quality by adding phenolic resin, phenyl siloxane rubber and organic fiber in softwood mix material.
The cork composite material of the present invention, is made up of following weight parts proportioning: cork particle 80～100, synvaren 5～20, phenyl siloxane rubber 2～15, organic fiber 0.5～5. Preferred cork particle 90～100, synvaren 10～20, phenyl siloxane rubber 4～12, organic fiber 1～4, under this proportioning cork composite material shock-resistant, heat-proof quality is high.
Described synvaren is the mixture of one or more in boron modified phenolic resin, ba phenolic resin or magnesium synvaren, adopts synvaren to improve thermostability.
Described phenyl siloxane rubber is one or both in methyl phenyl silicone rubber or methyl phenyl vinyl silicone rubber, preferred methyl phenyl silicone rubber.In preparation technology, methyl phenyl silicone rubber manufacturability is better.
The phenyl molar content of described phenyl siloxane rubber ranges for 5～40%, it is preferable that phenyl molar content ranges for 5～30%, within the scope of this phenyl content methyl phenyl silicone rubber be easily mixed, good manufacturability.
Described organic fiber is Fanglun 1313, Polyphenylene Sulfone nylon, gathers the mixture of one or more in benzimidazole fiber, polyhenylene pyrido diimidazole fiber, poly-p-phenylene-benzobisoxazole fiber, polyphenylene sulfide fibre, polyether ketone fiber, polyetheretherketonefiber fiber, polypyrrole fiber. Above-mentioned organic fiber good toughness, intensity are high, high temperature resistant, and the impact resistance of cork composite material is played a key effect.
The length range of described organic fiber is 5～30mm, it is preferable that length range is 5～10mm. Fiber in this length range is chopped strand, and good dispersion is not easily reunited.
A kind of preparation method of shock-resistant heat insulation cork composite material, concrete preparation process and condition are as follows:
(1) cork powder particle is sieved, filter out the cork particle that particle diameter is 30～60 orders;
(2) cork powder after screening being carried out heat treatment, heat treatment time is 5～30h, obtains the cork powder after heat treatment;
(3) by pretreated cork particle, modified phenolic adhesive, phenyl siloxane rubber, organic fiber mechanical agitation mix homogeneously, mixed material is obtained; Cork particle 80～100, synvaren 5～20, phenyl siloxane rubber 2～15, organic fiber 0.5～5;
(4) mixed material being put into mould, apply 1～10 ton of pressure, mould is placed on vulcanizer hot plate and solidifies, and solidification temperature is 100～200 DEG C, and hardening time is 1～12h;
(5) mould is taken out after terminating by solidification, is cooled to room temperature, and die sinking sampling obtains cork composite material.
Heat treatment described in step (2) is normal pressure drying, vacuum drying or 100～150 DEG C of steam treatment of high temperature.
Curing described in step (4) is isothermal curing or gradient increased temperature solidification.
Heat treatment described in step b) is normal pressure drying, vacuum drying or high temperature steam treatment;
Curing described in step d) can be isothermal curing or gradient increased temperature solidification, and wherein gradient increased temperature is solidified with the molding being beneficial to special-shaped structure piece, and solidification can be made more abundant, and performance is higher.
Present invention advantage compared with prior art is in that: cork composite material prepared by the present invention, and density is low, maintains good mechanical property. And the synergism by modified phenolic adhesive, phenyl siloxane rubber and organic fiber, overcome the problem that existing cork is heat-resisting and toughness is poor, make cork composite material have concurrently excellence thermal insulation and resistance to impact (thermal conductivity at the cork composite material of the present invention 150 DEG C ranges for 0.05～0.08W/m K, and impact strength ranges for 2.2～4.0kJ/m2; And the thermal conductivity at existing 301 trade mark cork composite material 150 DEG C ranges for 0.09～0.12W/m K, impact strength ranges for 0.6～1.0kJ/m2). Cork composite material preparation method technique provided by the invention is simple and is prone to regulation and control, it is not necessary to special process equipment, cost is low, has commercial introduction application value.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described, but does not constitute limiting the scope of the invention.
Embodiment 1
(1) with natural cork powder for raw material, the granulated cork that particle diameter is 30～60 orders is filtered out;
(2) weigh the above-mentioned granulated cork of 200g, be laid in container at 120 DEG C normal pressure and dry, take out after 24h;
(3) granulated cork after normal pressure drying and processing, boron modification modified phenolic adhesive, methyl phenyl silicone rubber (phenyl molar content is 20%) are carried out mechanical agitation mixing by proportion by weight 100:15:5, incorporation time is 30min, continuously add the Fanglun 1313 (length 5～10mm) that mass parts is 2 and mix 30min, obtain mixed material;
(4) said mixture material being put into mould, apply 5 tons of pressure, mould is placed on vulcanizer and carries out isothermal curing, and solidification temperature is 160 DEG C, and hardening time is 10h;
(5) mould is taken out after terminating by solidification, is cooled to room temperature, and die sinking sampling obtains cork composite material.
The cork composite material obtained is tested, and 150 DEG C of thermal conductivities are 0.08W/m K, and impact strength is 2.5kJ/m2。
Embodiment 2
(1) with natural cork powder for raw material, the granulated cork that particle diameter is 30～60 orders is filtered out;
(2) weigh the above-mentioned granulated cork of 200g, be laid in container at 100 DEG C normal pressure and dry, take out after 24h;
(3) granulated cork after normal pressure drying and processing, boron modification modified phenolic adhesive, methyl phenyl silicone rubber (phenyl molar content is 10%) are carried out mechanical agitation mixing by proportion by weight 100:14:8, incorporation time is 50min, continuously add mass parts be 1.8 poly-benzimidazole fiber (length 5～10mm) is mixed 60min, obtain mixed material;
(4) said mixture material being put into mould, apply 10 tons of pressure, mould is placed on vulcanizer and carries out isothermal curing, and solidification temperature is 180 DEG C, and hardening time is 6h;
(5) mould is taken out after terminating by solidification, is cooled to room temperature, and die sinking sampling obtains cork composite material.
The cork composite material obtained is tested, and 150 DEG C of thermal conductivities are 0.08W/m K, and impact strength is 2.2kJ/m2。
Embodiment 3
(1) with natural cork powder for raw material, the granulated cork that particle diameter is 30～60 orders is filtered out;
(2) weigh the above-mentioned granulated cork of 200g, be laid in container at 100 DEG C vacuum drying, take out after 12h;
(3) granulated cork after being processed by vacuum drying, boron modification modified phenolic adhesive, methyl phenyl vinyl silicone rubber (phenyl molar content is 15%) carry out mechanical agitation mixing by proportion by weight 80:12:5, incorporation time is 30min, continuously add polyhenylene pyrido diimidazole fiber (length 5～10mm) that mass parts is 2 and mix 40min, obtain mixed material;
(4) said mixture material being put into mould, apply 5 tons of pressure, mould is placed on vulcanizer and carries out gradient increased temperature solidification, the first stage: solidify 6h at 120 DEG C, second stage: solidify 4h at 180 DEG C;
(5) mould is taken out after terminating by solidification, is cooled to room temperature, and die sinking sampling obtains cork composite material.
The cork composite material obtained is tested, and 150 DEG C of thermal conductivities are 0.07W/m K, and impact strength is 2.8kJ/m2。
Embodiment 4
(1) with natural cork powder for raw material, the granulated cork that particle diameter is 30～60 orders is filtered out;
(2) weigh the above-mentioned granulated cork of 200g, be laid in container at 120 DEG C vacuum drying, take out after 8h;
(3) granulated cork after being processed by vacuum drying, boron modification modified phenolic adhesive, methyl phenyl silicone rubber (phenyl molar content is 5%) carry out mechanical agitation mixing by proportion by weight 90:13:9, incorporation time is 30min, continuously add the polyetheretherketonefiber fiber (length 5～10mm) that mass parts is 2.2 and mix 60min, obtain mixed material;
(4) said mixture material being put into mould, apply 8 tons of pressure, mould is placed on vulcanizer and carries out gradient increased temperature solidification, the first stage: solidify 4h at 150 DEG C, second stage: solidify 4h at 180 DEG C;
(5) mould is taken out after terminating by solidification, is cooled to room temperature, and die sinking sampling obtains cork composite material.
The cork composite material obtained is tested, and 150 DEG C of thermal conductivities are 0.08W/m K, and impact strength is 3.0kJ/m2。
Embodiment 5
(1) with natural cork powder for raw material, the granulated cork that particle diameter is 30～60 orders is filtered out;
(2) weigh the above-mentioned granulated cork of 200g, be laid in container at 120 DEG C normal pressure and dry, take out after 24h;
(3) granulated cork after normal pressure drying and processing, boron modification modified phenolic adhesive, methyl phenyl silicone rubber (phenyl molar content is 30%) are carried out mechanical agitation mixing by proportion by weight 100:16:6, incorporation time is 45min, continuously add the Fanglun 1313 (length 5～10mm) that mass parts is 2.0 and mix 60min, obtain mixed material;
(4) said mixture material being put into mould, apply 10 tons of pressure, mould is placed on vulcanizer and carries out gradient increased temperature solidification, the first stage: solidify 3h at 120 DEG C, second stage: solidify 3h at 150 DEG C, the phase III: solidify 2h at 180 DEG C; ;
(5) mould is taken out after terminating by solidification, is cooled to room temperature, and die sinking sampling obtains cork composite material.
The cork composite material obtained is tested, and 150 DEG C of thermal conductivities are 0.07W/m K, and impact strength is 3.4kJ/m2。
Embodiment 6
(1) with natural cork powder for raw material, the granulated cork that particle diameter is 30～60 orders is filtered out;
(2) weigh the above-mentioned granulated cork of 200g, be laid in container at 120 DEG C normal pressure and dry, take out after 24h;
(3) granulated cork after normal pressure drying and processing, boron modification modified phenolic adhesive, methyl phenyl vinyl silicone rubber (phenyl molar content is 5%) are carried out mechanical agitation mixing by proportion by weight 100:10:10, incorporation time is 60min, continuously add the polyphenylene sulfide fibre (length 5～10mm) that mass parts is 3.5 and mix 60min, obtain mixed material;
(4) said mixture material being put into mould, apply 10 tons of pressure, mould is placed on vulcanizer and carries out gradient increased temperature solidification, the first stage: solidify 4h at 120 DEG C, second stage: solidify 5h at 150 DEG C;
(5) mould is taken out after terminating by solidification, is cooled to room temperature, and die sinking sampling obtains cork composite material.
The cork composite material obtained is tested, and 150 DEG C of thermal conductivities are 0.08W/m K, and impact strength is 3.6kJ/m2。
Embodiment 7
(1) with natural cork powder for raw material, the granulated cork that particle diameter is 30～60 orders is filtered out;
(2) weigh the above-mentioned granulated cork of 200g, be laid in container at 150 DEG C normal pressure and dry, take out after 5h;
(3) granulated cork after normal pressure drying and processing, boron modification modified phenolic adhesive, methyl phenyl silicone rubber (phenyl molar content is 20%) are carried out mechanical agitation mixing by proportion by weight 100:18:11, incorporation time is 90min, continuously add the Fanglun 1313 (length 5～10mm) that mass parts is 1.5 and mix 60min, obtain mixed material;
(4) said mixture material being put into mould, apply 5 tons of pressure, mould is placed on vulcanizer and carries out isothermal curing, and solidification temperature is 180 DEG C, and hardening time is 12h;
(5) mould is taken out after terminating by solidification, is cooled to room temperature, and die sinking sampling obtains cork composite material.
The cork composite material obtained is tested, and 150 DEG C of thermal conductivities are 0.05W/m K, and impact strength is 3.5kJ/m2。
Embodiment 8
(1) with natural cork powder for raw material, the granulated cork that particle diameter is 30～60 orders is filtered out;
(2) weigh the above-mentioned granulated cork of 200g, be laid in container at 100 DEG C normal pressure and dry, take out after 30h;
(3) granulated cork after normal pressure drying and processing, boron modification modified phenolic adhesive, methyl phenyl silicone rubber (phenyl molar content is 24%) are carried out mechanical agitation mixing by proportion by weight 100:10:12, incorporation time is 90min, continuously add the polyetheretherketonefiber fiber (length 5～10mm) that mass parts is 3.8 and mix 60min, obtain mixed material;
(4) said mixture material being put into mould, apply 10 tons of pressure, mould is placed on vulcanizer and carries out gradient increased temperature solidification, the first stage: solidify 2h at 120 DEG C, second stage: solidify 3h at 150 DEG C, the phase III: solidify 4h at 180 DEG C; ;
(5) mould is taken out after terminating by solidification, is cooled to room temperature, and die sinking sampling obtains cork composite material.
The cork composite material obtained is tested, and 150 DEG C of thermal conductivities are 0.06W/m K, and impact strength is 4.0kJ/m2。
Claims (10)
1. a shock-resistant heat insulation cork composite material, it is characterised in that: its weight consists of:
Cork particle 80～100, synvaren 5～20, phenyl siloxane rubber 2～15, organic fiber 0.5～5.
2. the shock-resistant heat insulation cork composite material of one according to claim 1, it is characterised in that: described cork particle 90～100, synvaren 10～20, phenyl siloxane rubber 4～12, organic fiber 1～4.
3. the shock-resistant heat insulation cork composite material of one according to claim 1 and 2, it is characterised in that: described synvaren is the mixture of one or more in boron modified phenolic resin, ba phenolic resin or magnesium synvaren.
4. the shock-resistant heat insulation cork composite material of one according to claim 1 and 2, it is characterised in that: described phenyl siloxane rubber is one or both in methyl phenyl silicone rubber or methyl phenyl vinyl silicone rubber. Preferred methyl phenyl silicone rubber.
5. the shock-resistant heat insulation cork composite material of one according to claim 1 and 2, it is characterised in that: the phenyl molar content of described phenyl siloxane rubber ranges for 5～40%, it is preferable that phenyl molar content ranges for 5～30%.
6. the shock-resistant heat insulation cork composite material of one according to claim 1, it is characterised in that: described organic fiber is Fanglun 1313, Polyphenylene Sulfone nylon, gathers the mixture of one or more in benzimidazole fiber, polyhenylene pyrido diimidazole fiber, poly-p-phenylene-benzobisoxazole fiber, polyphenylene sulfide fibre, polyether ketone fiber, polyetheretherketonefiber fiber, polypyrrole fiber.
7. the shock-resistant heat insulation cork composite material of one according to claim 1 or 6, it is characterised in that: the length range of described organic fiber is 5～30mm, it is preferable that length range is 5～10mm.
8. the preparation method of a shock-resistant heat insulation cork composite material, it is characterised in that: concrete preparation process and condition are as follows:
(1) cork powder particle is sieved, filter out the cork particle that particle diameter is 30～60 orders;
(2) cork powder after screening being carried out heat treatment, heat treatment time is 5～30h, obtains the cork powder after heat treatment;
(3) by pretreated cork particle, modified phenolic adhesive, phenyl siloxane rubber, organic fiber mechanical agitation mix homogeneously, mixed material is obtained; Cork particle 80～100, synvaren 5～20, phenyl siloxane rubber 2～15, organic fiber 0.5～5;
(4) mixed material being put into mould, apply 1～10 ton of pressure, mould is placed on vulcanizer hot plate and solidifies, and solidification temperature is 100～200 DEG C, and hardening time is 1～12h;
(5) mould is taken out after terminating by solidification, is cooled to room temperature, and die sinking sampling obtains cork composite material.
9. the preparation method of cork composite material according to claim 8, it is characterised in that: the heat treatment described in step (2) is normal pressure drying, vacuum drying or 100～150 DEG C of steam treatment of high temperature.
10. the preparation method of cork composite material according to claim 8, it is characterised in that: the curing described in step (4) is isothermal curing or gradient increased temperature solidification.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN110396365A (en) * | 2019-06-27 | 2019-11-01 | 航天材料及工艺研究所 | Flexible protective layer, cork composite material structure with flexible protective layer and preparation method thereof |
| CN113700710A (en) * | 2021-08-25 | 2021-11-26 | 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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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110396365A (en) * | 2019-06-27 | 2019-11-01 | 航天材料及工艺研究所 | Flexible protective layer, cork composite material structure with flexible protective layer and preparation method thereof |
| 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 |
| CN113700710A (en) * | 2021-08-25 | 2021-11-26 | 湖北三江航天红阳机电有限公司 | Method for sticking cork wood |
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