CN107828096A - A kind of high-elongation butyronitrile of resistance to ablation thermal insulation layer material and its manufacture method - Google Patents
A kind of high-elongation butyronitrile of resistance to ablation thermal insulation layer material and its manufacture method Download PDFInfo
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- CN107828096A CN107828096A CN201711136355.3A CN201711136355A CN107828096A CN 107828096 A CN107828096 A CN 107828096A CN 201711136355 A CN201711136355 A CN 201711136355A CN 107828096 A CN107828096 A CN 107828096A
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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
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/02—Copolymers with acrylonitrile
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
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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 provides a kind of high-elongation butyronitrile of resistance to ablation thermal insulation layer material and its manufacture method, the high-elongation butyronitrile of the resistance to ablation thermal insulation layer material of preparation, in parts by weight, including 100~102 parts of nitrile rubber, 1.5~3 parts of stearic acid, 5~8 parts of zinc oxide, 8~10 parts of carborundum, 20~25 parts of boron bakelite resin, 20~30 parts of deca-BDE, 10~15 parts of antimony oxide, 15~20 parts of white carbon, 3~5 parts of 10~20 parts of di-n-octyl sebacate, 5~8 parts of aramid short fiber and cumyl peroxide.The present invention uses cumyl peroxide vulcanizing system, improves the mechanical property and ablation property of nitrile rubber heat insulation layer by adding the material such as white carbon and feature phenolic resin, realizes the high-elongation and ablation resistance of nitrile rubber heat insulation layer.
Description
Technical field
The present invention relates to solar heat protection thermal insulation layer material in a kind of Solid Rocket Motor combustion chamber, is also applied for structural type thermal insulation
Layer, such as pulsed motor soft spacer, advance tactics cover.
Background technology
Heat insulation layer is the pith of thermal protection struc ture in solid propellant rocket, and playing prevents in motor combustion chamber case
Temperature, which reaches, jeopardizes self structure integrality, carries resistance high temperature, high combustion gas stream and the effect of particulate matter erosion.For structure
Type heat insulation layer also plays security isolation propellant, protects the improper important function lighted of propellant.Common adiabatic layer material
Mainly there is EPDM rubber insulation, nitrile rubber heat insulation layer and rubber/fiber composite thermal insulation layer material etc..With rocket,
The development of missilery, the performance requirement of adiabatic layer material is except with good solar heat protection ablation resistance, and to heat insulation layer
Structuring application propose higher requirement.Heat insulation layer is no longer single entirety, because needing for structure may be divided into
If stem portion, it is bonded and integrated by local, it is desirable to which heat insulation layer can not only play the effect of solar heat protection anti-yaw damper, additionally it is possible to bear
The large deformation that propellant is pressurized or combustion gas work is brought, that is, need higher mechanical property.
Ethylene propylene diene rubber is because its heat decomposition temperature is high, and thermal decomposition heat absorption is big, and heatproof air aging performance is good, volumetric efficiency
Greatly, there is good compatibility with a variety of propellants and housing composite, be heat-insulating material in the preferable housing of engine, but
Be EPDM polarity it is low, adhesive property is poor, limits its structuring application power.Nitrile rubber heat insulation layer has higher
Polarity, impart it compared with excellent adhesion property, be better than EPDM rubber insulation in structuring application aspect, but its is resistance to
Ablative and mechanical property is relatively low.
Application of the adiabatic layer material of composite construction in solid propellant rocket is less, it is desirable to the ablation resistance of heat insulation layer
Energy, mechanical property and adhesive property three can meet structuring requirement, and by contrast, nitrile rubber ablation property is less than ternary
EP rubbers, mechanical property difference unobvious, but adhesive property is more excellent.
In addition, common sulfur vulcanized rubber system, easily has the risk of material calcination, the performance of material is influenceed.
The content of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of high-elongation butyronitrile of resistance to ablation thermal insulation layer material, adopted
With cumyl peroxide vulcanizing system, improve nitrile rubber thermal insulation by adding the material such as white carbon and feature phenolic resin
The mechanical property and ablation property of layer, realize the high-elongation and ablation resistance of nitrile rubber heat insulation layer.
The technical solution adopted for the present invention to solve the technical problems is：
The heat insulation layer material prescription of the present invention is as follows：A kind of high-elongation butyronitrile of resistance to ablation thermal insulation layer material, with parts by weight
Meter, including following component：100~102 parts of nitrile rubber, 1.5~3 parts of stearic acid, 5~8 parts of zinc oxide, 8~10 parts of carborundum,
20~25 parts of boron bakelite resin, 20~30 parts of deca-BDE, 10~15 parts of antimony oxide, 15~20 parts of white carbon, the last of the ten Heavenly stems two
3~5 parts of 10~20 parts of dioctyl phthalate, 5~8 parts of aramid short fiber and cumyl peroxide.
The present invention also provides the preparation method of the above-mentioned high-elongation butyronitrile of resistance to ablation thermal insulation layer material, comprises the following steps：
1) aramid short fiber and white carbon are dried into 1h at 80 DEG C；
2) by the nitrile rubber of 100~102 parts by weight in thin logical 5~8 times in mill；
3) successively by 5~8 part by weight of zinc oxide, 1.5~3 parts by weight stearic acid, 8~10 parts by weight carborundum, 20~25
Parts by weight boron bakelite resin, 20~30 parts by weight deca-BDEs, 10~15 parts by weight antimony oxides add nitrile rubber, roller
Rolled 3 times away from glue for 3mm, is cut；
4) 15~20 parts by weight white carbons and 10~20 parts by weight di-n-octyl sebacates are added several times, roll spacing 3mm, are cut
Glue rolls 3 times；
5) 5~8 parts by weight aramid short fibers are added several times, are cut glue and are rolled 3 times, roll spacing 3mm；
6) it is thin logical 2 times, roll spacing 0.3mm；Then at roll spacing 3mm, cut glue and roll 2 times；Repeat this step 3 times；
7) cumyl peroxide of 3~5 parts by weight is added, roll spacing 3mm, glue is cut and rolls 2 times；
8) it is thin logical 2 times, roll spacing 0.3mm；Then at roll spacing 3mm, cut glue and roll 2 times；Repeat this step 2 times；
9) roll spacing 6mm~7mm slices, cooling are placed；
10) after standing 24h, back mixing is carried out；It is thin logical 2 times, roll spacing 0.3mm；Then at roll spacing 3mm, cut glue and roll 2 times；Weight
Duplicate step 2 time；
11) slice, 60~70min, 5~12MPa of pressure are vulcanized at 160 DEG C ± 2 DEG C.
The beneficial effects of the invention are as follows：The nitrile rubber heat insulation layer performance of preparation is in terms of mechanical property and ablation resistance
Positive effect is improved, specifically see the table below：
The resistance to ablation ability of heat insulation layer is embodied in the carbon forming rate of material, and carbon forming rate is largely decided by be used
Resin, Carbonized structure uniformly, fine and close and high carbon-coating intensity, can effectively resist washing away for air-flow and particulate matter,
Protective effect is served to carbonization part.The present invention has high carbon content, high arylation, macromolecule using boron bakelite resin
The design feature of amount and high crosslink density, carbon forming rate is high, and heat-resisting quantity is good, is the important materials for improving carbon-coating quality.White carbon
It is the main reinforced filling of rubber, its reinforcement mechanism is commonly considered as that silica particles are small, and specific surface area is big, indirectly with rubber
Contacting surface product is more, forms substantial amounts of chemical interface, plays the role of to the mechanical property of material important.In addition, reasonably refine work
Skill has certain influence to stability, the uniformity of material property.
Embodiment
With reference to embodiment, the present invention is further described, and the present invention includes but are not limited to following embodiments.
The heat insulation layer material prescription of the present invention is as follows：
| Sequence number | Recipe ingredient title | Recipe ingredient matches (weight) | Remarks |
| 1 | Nitrile rubber | 100~102 | Matrix |
| 2 | Stearic acid | 1.5~3.0 | Accelerator |
| 3 | Zinc oxide | 5~8 | Accelerator |
| 4 | Carborundum | 8~10 | Reinforcing agent |
| 5 | Boron bakelite resin | 20~25 | The filler of resistance to ablation |
| 6 | Deca-BDE | 20~30 | The filler of resistance to ablation, heat-resistant agent |
| 7 | Antimony oxide | 10~15 | Fire retardant |
| 8 | White carbon | 15~20 | Fire retardant |
| 9 | Di-n-octyl sebacate | 10~20 | The filler of resistance to ablation, reinforcing agent |
| 10 | Aramid short fiber | 5~8 | Plasticiser |
| 11 | Cumyl peroxide | 3~5 | Vulcanizing agent |
The preparation technology flow of the adiabatic layer material of the present invention is：
1) according to ratio, dispensing；
2) load weighted aramid short fiber, white carbon are dried into 1h at 80 DEG C；
3) by load weighted nitrile rubber, lead to 5 times~8 times in thin in mill；
4) zinc oxide, stearic acid, carborundum, boron bakelite resin, deca-BDE, antimony oxide are added into butyronitrile successively
Rubber, roll spacing 3mm；Glue is cut to roll 3 times；
5) white carbon and di-n-octyl sebacate, roll spacing 3mm are added several times；Glue is cut to roll 3 times；
6) aramid short fiber is added several times, is cut glue and is rolled 3 times, roll spacing 3mm；
7) it is thin logical 2 times, roll spacing 0.3mm, then at roll spacing 3mm, cut glue and roll 2 times；Repeat the step 3 times；
8) cumyl peroxide is added, roll spacing 3mm, glue is cut and rolls 2 times；
9) it is thin logical 2 times, roll spacing 0.3mm, then at roll spacing 3mm, cut glue and roll 2 times；Repeat the step 2 times；
10) roll spacing is beaten and placed in 6mm~7mm slices, cooling；
11) after standing 24h, back mixing is carried out.It is thin logical 2 times, roll spacing 0.3mm, then at roll spacing 3mm, cut glue and roll 2 times；Weight
Step 2 times again；
12) slice, performance test test specimen is made.160 DEG C ± 2 DEG C of curing temperature, time 60min~70min, pressure 5MPa
~12MPa (related to vulcanizing press and mould).
Example 1
(1) formula each component is weighed
Formula each component is weighed according to following table.
(2) heat insulation layer is refined
A) load weighted aramid short fiber, white carbon are dried into 1h at 80 DEG C；
B) by nitrile rubber, lead to 5 times~8 times in thin in mill；
C) zinc oxide, stearic acid, carborundum, boron bakelite resin, deca-BDE, antimony oxide, roll spacing are sequentially added
For 3mm；Glue is cut to roll 3 times；
D) divide 3 times and add white carbon and di-n-octyl sebacate, roll spacing 3mm；Glue is cut to roll 3 times；
E) divide 5 addition aramid short fibers, cut glue and roll 3 times, roll spacing 3mm；
F) it is thin logical 2 times, roll spacing 0.3mm, then at roll spacing 3mm, cut glue and roll 2 times；Repeat the step 3 times；
G) cumyl peroxide is added, roll spacing 3mm, glue is cut and rolls 2 times；
H) it is thin logical 2 times, roll spacing 0.3mm, then at roll spacing 3mm, cut glue and roll 2 times；Repeat the step 2 times；
I) slice, cooling are placed；
J) after standing 24h, back mixing.It is thin logical 2 times, roll spacing 0.3mm, then at roll spacing 3mm, cut glue and roll 2 times；Repeat the step
2 times；
K) slice, performance test test specimen is made.160 DEG C, time 60min, pressure 10MPa of curing temperature.
(3) performance test
Refined heat insulation layer material properties test result is as follows：
Example 2
(1) formula each component is weighed
Formula each component is weighed according to following table.
(2) heat insulation layer is refined
A) load weighted aramid short fiber, white carbon are dried into 1h at 80 DEG C；
B) by nitrile rubber, lead to 5 times~8 times in thin in mill；
C) zinc oxide, stearic acid, carborundum, boron bakelite resin, deca-BDE, antimony oxide, roll spacing are sequentially added
For 3mm；Glue is cut to roll 3 times；
D) divide 3 times and add white carbon and di-n-octyl sebacate, roll spacing 3mm；Glue is cut to roll 3 times；
E) divide 5 addition aramid short fibers, cut glue and roll 3 times, roll spacing 3mm；
F) it is thin logical 2 times, roll spacing 0.3mm, then at roll spacing 3mm, cut glue and roll 2 times；Repeat the step 3 times；
G) cumyl peroxide is added, roll spacing 3mm, glue is cut and rolls 2 times；
H) it is thin logical 2 times, roll spacing 0.3mm, then at roll spacing 3mm, cut glue and roll 2 times；Repeat the step 2 times；
I) slice, cooling are placed；
J) after standing 24h, back mixing.It is thin logical 2 times, roll spacing 0.3mm, then at roll spacing 3mm, cut glue and roll 2 times；Repeat the step
2 times；
K) slice, performance test test specimen is made.160 DEG C, time 65min, pressure 10MPa of curing temperature.
(3) performance test
Refined heat insulation layer material properties test result is as follows：
Example 3
(1) formula each component is weighed
Formula each component is weighed according to following table.
(2) heat insulation layer is refined
A) load weighted aramid short fiber, white carbon are dried into 1h at 80 DEG C；
B) by nitrile rubber, lead to 5 times~8 times in thin in mill；
C) zinc oxide, stearic acid, carborundum, boron bakelite resin, deca-BDE, antimony oxide, roll spacing are sequentially added
For 3mm；Glue is cut to roll 3 times；
D) divide 3 times and add white carbon and di-n-octyl sebacate, roll spacing 3mm；Glue is cut to roll 3 times；
E) divide 5 addition aramid short fibers, cut glue and roll 3 times, roll spacing 3mm；
F) it is thin logical 2 times, roll spacing 0.3mm, then at roll spacing 3mm, cut glue and roll 2 times；Repeat the step 3 times；
G) cumyl peroxide is added, roll spacing 3mm, glue is cut and rolls 2 times；
H) it is thin logical 2 times, roll spacing 0.3mm, then at roll spacing 3mm, cut glue and roll 2 times；Repeat the step 2 times；
I) slice, cooling are placed；
J) after standing 24h, back mixing.It is thin logical 2 times, roll spacing 0.3mm, then at roll spacing 3mm, cut glue and roll 2 times；Repeat the step
2 times；
K) slice, performance test test specimen is made.160 DEG C, time 65min, pressure 10MPa of curing temperature.
(3) performance test
Refined heat insulation layer material properties test result is as follows：
Claims (2)
- A kind of 1. high-elongation butyronitrile of resistance to ablation thermal insulation layer material, it is characterised in that in parts by weight, including following component：100~102 parts of nitrile rubber, 1.5~3 parts of stearic acid, 5~8 parts of zinc oxide, 8~10 parts of carborundum, boron bakelite resin 20 ~25 parts, 20~30 parts of deca-BDE, 10~15 parts of antimony oxide, 15~20 parts of white carbon, di-n-octyl sebacate 10~ 20 parts, 3~5 parts of 5~8 parts of aramid short fiber and cumyl peroxide.
- A kind of 2. manufacture method of the high-elongation butyronitrile of resistance to ablation thermal insulation layer material described in claim 1, it is characterised in that including Following step：1) aramid short fiber and white carbon are dried into 1h at 80 DEG C；2) by the nitrile rubber of 100~102 parts by weight in thin logical 5~8 times in mill；3) successively by 5~8 part by weight of zinc oxide, 1.5~3 parts by weight stearic acid, 8~10 parts by weight carborundum, 20~25 weight Part boron bakelite resin, 20~30 parts by weight deca-BDEs, 10~15 parts by weight antimony oxides add nitrile rubber, and roll spacing is 3mm, cut glue and roll 3 times；4) 15~20 parts by weight white carbons and 10~20 parts by weight di-n-octyl sebacates are added several times, roll spacing 3mm, are cut glue and are turned over Rolling 3 times；5) 5~8 parts by weight aramid short fibers are added several times, are cut glue and are rolled 3 times, roll spacing 3mm；6) it is thin logical 2 times, roll spacing 0.3mm；Then at roll spacing 3mm, cut glue and roll 2 times；Repeat this step 3 times；7) cumyl peroxide of 3~5 parts by weight is added, roll spacing 3mm, glue is cut and rolls 2 times；8) it is thin logical 2 times, roll spacing 0.3mm；Then at roll spacing 3mm, cut glue and roll 2 times；Repeat this step 2 times；9) roll spacing 6mm~7mm slices, cooling are placed；10) after standing 24h, back mixing is carried out；It is thin logical 2 times, roll spacing 0.3mm；Then at roll spacing 3mm, cut glue and roll 2 times；Repeat this Step 2 time；11) slice, 60~70min, 5~12MPa of pressure are vulcanized at 160 DEG C ± 2 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109942917A (en) * | 2019-03-27 | 2019-06-28 | 赛兴(北京)科技有限公司 | A kind of carborundum powder enhancing high-performance rubber material and preparation method thereof |
| CN112625318A (en) * | 2020-12-16 | 2021-04-09 | 湖北航天化学技术研究所 | Environment-friendly ablation-resistant rubber type heat-insulating layer and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109942917A (en) * | 2019-03-27 | 2019-06-28 | 赛兴(北京)科技有限公司 | A kind of carborundum powder enhancing high-performance rubber material and preparation method thereof |
| CN112625318A (en) * | 2020-12-16 | 2021-04-09 | 湖北航天化学技术研究所 | Environment-friendly ablation-resistant rubber type heat-insulating layer and preparation method thereof |
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Application publication date: 20180323 |