CN108084714A - A kind of preparation method of the resistance to ablative insulative material of silicon rubber - Google Patents
A kind of preparation method of the resistance to ablative insulative material of silicon rubber Download PDFInfo
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- CN108084714A CN108084714A CN201711488208.2A CN201711488208A CN108084714A CN 108084714 A CN108084714 A CN 108084714A CN 201711488208 A CN201711488208 A CN 201711488208A CN 108084714 A CN108084714 A CN 108084714A
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- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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Abstract
The present invention relates to a kind of preparation methods of the resistance to ablative insulative material of silicon rubber, belong to heat-insulating material technical field.The present invention with polyimide resin by disperseing compound with tantalum oxide coagulant liquid in a solvent and coating to silastic material surface; due to having well into charcoal in polyimide material; applied in silicone rubber matrix; the linear ablative rate of material can be reduced; have simultaneously by polyimides excellent into carbon, it made to form protective film after heated charing, effectively reduce heat further deeply; material is prevented to continue ablation, improves the ablation resistance of material；And the present invention uses tantalum oxide as modified material; it is being carbonized by an aqueous precursor gel part under thermal ablation and is being compounded to form ramet clad with tantalum oxide gel; since carbonization tantalum material has excellent physical and chemical properties, preferable inoxidizability resistant to chemical etching and high thermal shock resistance properties; make it as the resistance to ablative shielding of high temperature, effectively improve the ablation resistance of material.
Description
Technical field
The present invention relates to a kind of preparation methods of the resistance to ablative insulative material of silicon rubber, belong to heat-insulating material technical field.
Background technology
Adiabatic layer material can substantially be divided into three types：1. subliming type heat-insulating material.This heat-insulating material is with stone mostly
Ink material and carbon/carbon compound material can distil, due to distillation to represent material when flame vigorous combustion is in such material
Substantial amounts of calory burning is taken away in heat absorption；Moreover, subliming type heat-insulating material has very big heat emissivity coefficient, there is good heat resistance
Energy.But the thermal insulation of ablation layer is poor after ablation and such material price is expensive, limits its application in a wider context.
2. thawing type heat-insulating material.This heat-insulating material is using glass, quartz and silica-base material as material is represented mostly, such material exists
It is melted rapidly in ablation environment, absorbs substantial amounts of heat；Meanwhile SiO can be formed after thawing effect occurs2Liquid is protected
Film can resist washing away for high-temperature high-speed airflow, but thawing type heat-insulating material is unfavorable for producing on a large scale.3. carbonization type is exhausted
Thermosphere material.Such heat-insulating material is mainly using resin or elastomer as main basis material, based on fiber or fiber cloth
The reinforcing material wanted absorbs the heat of combustion chambers burn using carbonization of the two phase material after ablation is reacted, while material passes through
Carburization zone is formed after ablation, reaches solar heat protection purpose using carburization zone heat loss through radiation.
It using carbon is matrix, carbon fiber for reinforcing material that the adiabatic layer material of carbon/carbon-based, which is, passes through a series of working processes and carbon
Change handles to obtain full carbonaceous composite material, and carbon content is up to more than 99% after high-temperature process.Basis material mainly has pyrolytic carbon
With two kinds of impregnated carbon.Reinforcing material refers mainly to the carbon fiber for having high-modulus, high intensity, coefficient of thermal expansion low.Prepare composite wood
Green body first generally is made by the methods of winding, molding, stacking, establishment in carbon fiber during material, adhesive is made by fiber with resin
It is bonded on basis material, densification is then carried out by chemical vapour deposition technique or high hydraulic pressure phase infusion process, formed
Deposited carbon layer.So carbon/carbon-based adiabatic layer material is removed with density is small, mechanical behavior under high temperature is good, wear resistance is excellent
Outside feature, ablation resistance is fine, is ideal adiabatic layer material.In recent years, domestic and foreign scholars are to carbon/carbon-based heat insulation layer
Material mixes dystectic ceramic material, substantially increases its ablation resistance.But existing resistance to ablative insulative material heat is surely
Qualitative poor, heat-insulating material charring layer consolidation is poor, phenomena such as easily fracture, so it is preferable to prepare a kind of thermal stability
Resistance to ablative insulative material be prior art the most important thing.
The content of the invention
The technical problems to be solved by the invention：For Heat Conduction Material in use, long-time heat conduction processing makes it
The problem of changing with volume stability easily is expanded, provides a kind of preparation side of low expansion high heat conduction carbon composite
Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）In mass ratio 1：5, polyimide resin is added in n,N-dimethylacetamide, mixed liquor is obtained and is stirred,
N,N-dimethylacetamide dilution processing is added dropwise, obtains dilution；
（2）In mass ratio 1:10, tantalic chloride is added in absolute ethyl alcohol, is stirred to obtain lysate and by volume 1:10,
Glucose solution is added dropwise in lysate, after being added dropwise to complete, is stirred and stands, obtain modification liquid；
（3）It counts in parts by weight, weighs 45~50 parts of modification liquids, 10~15 parts of aqueous povidone solutions and 1~2 respectively
Part propylene oxide is placed in three-necked flask, is stirred to obtain coagulant liquid, and by volume 1:5, dilution is added in coagulant liquid,
Simultaneously heating water bath is stirred, after standing 40~48h, obtains standing liquid；
（4）Liquid rotary evaporation will be stood, concentrated gel liquid is obtained, tantalum oxide is taken to be placed in ball grinder, ball milling sieves to obtain ball milling powder
End, then in mass ratio 1:15, ball-milled powder and concentrated gel liquid are stirred simultaneously ultrasonic disperse, obtain modified dispersion liquid；
（5）It counts in parts by weight, weighs 55~60 parts of silicon rubber, 10~15 parts of modified dispersion liquids, 2~3 parts of accelerating agents respectively
TMTD, 1~2 part of Cure of Rubber agent DBTU and 6~8 parts of white carbons are placed in open mill, are kneaded uniformly and are collected rubber compound, will be mixed
Rubber alloy is placed under vulcanizing press, and vulcanizing treatment, standing is cooled to room temperature, you can is prepared into a kind of silicon rubber heat insulating material of resistance to ablation
Material.
Step（2）The glucose solution drop rate is 2mL/min.
Step（4）The rotating evaporation temperature is 45~50 DEG C.
Step（5）The vulcanizing treatment condition is in 5~8MPa, 155~170 DEG C of vulcanizing treatments.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention with polyimide resin by disperseing compound with tantalum oxide coagulant liquid in a solvent and coating to silicon rubber material
Expect surface, due to having well into charcoal in polyimide material, burnt applied to the line that material in silicone rubber matrix, can be reduced
Erosion rate, while have by polyimides excellent into carbon, it is made to form protective film after heated charing, effectively reduces heat
Further deeply, material is prevented to continue ablation, improves the ablation resistance of material；
（2）The present invention uses tantalum oxide as modified material, and ablation occurs in high temperature environments by it, forms ramet, due to
Carbonization load is a kind of outstanding transition metal carbide, is being carbonized by an aqueous precursor gel part under thermal ablation and is being coagulated with tantalum oxide
Glue is compounded to form ramet clad, since carbonization tantalum material has excellent physical and chemical properties, the corruption of preferable chemically-resistant
Erosion and the high inoxidizability of thermal shock resistance properties make it as the resistance to ablative shielding of high temperature, effectively improve the ablation resistance of material.
Specific embodiment
In mass ratio 1：5, polyimide resin is added in n,N-dimethylacetamide, mixed liquor is obtained and stirs mixed
It closes, n,N-dimethylacetamide dilution processing is added dropwise, obtains dilution；In mass ratio 1:10, tantalic chloride is added to absolute ethyl alcohol
In, it is stirred to obtain lysate and by volume 1:10,5% glucose solution of mass fraction is added dropwise in lysate, is controlled
Drop rate processed is 2mL/min, after being added dropwise to complete, is stirred and stands 25~30min and obtain modification liquid, in parts by weight
Meter weighs 45~50 parts of modification liquids, 10~15 parts of 1% aqueous povidone solutions of mass fraction and 1~2 part of epoxy respectively
Propane is placed in three-necked flask, is stirred to obtain coagulant liquid, and by volume 1:5, dilution is added in coagulant liquid, stirring is mixed
Merging is placed in 10~12h of heating water bath at 55~65 DEG C, after standing 40~48h, obtains standing liquid, then rotates and steam at 45~50 DEG C
The 1/5 of standing liquid product is sent to, obtains concentrated gel liquid；Tantalum oxide is taken to be placed in ball grinder, the ball milling under 250~300r/min
3~5h crosses 200 mesh sieves and obtains ball-milled powder, and then in mass ratio 1:15, ball-milled powder and concentrated gel liquid are stirred juxtaposition
10~15min of ultrasonic disperse under 200~300W obtains modified dispersion liquid；It counts in parts by weight, weighs 55~60 parts of silicon rubbers respectively
Glue, 10~15 parts of modified dispersion liquids, 2~3 parts of Vulcanization accelerator TMTDs, 1~2 part of Cure of Rubber agent DBTU and 6~8 parts of white carbons are placed in
In open mill, it is kneaded uniformly and collects rubber compound, epoxy glue is placed under vulcanizing press, at 5~8MPa, 155~170 DEG C
100~120min of vulcanizing treatment, standing are cooled to room temperature, you can are prepared into a kind of resistance to ablative insulative material of silicon rubber.
Example 1
In mass ratio 1：5, polyimide resin is added in n,N-dimethylacetamide, mixed liquor is obtained and is stirred, is dripped
N,N-dimethylacetamide dilution is added to handle, obtains dilution；In mass ratio 1:10, tantalic chloride is added in absolute ethyl alcohol, is stirred
It mixes and mixes to obtain lysate and by volume 1:10,5% glucose solution of mass fraction is added dropwise in lysate, control is added dropwise
Rate is 2mL/min, after being added dropwise to complete, is stirred and stands 25min and obtain modification liquid, counts, weigh respectively in parts by weight
45 parts of modification liquids, 10 parts of 1% aqueous povidone solutions of mass fraction and 1 part of propylene oxide are placed in three-necked flask, are stirred
It mixes and mixes to obtain coagulant liquid, by volume 1:5, dilution is added in coagulant liquid, is stirred and is placed in water-bath at 55 DEG C and adds
Hot 12h after standing 40h, obtains standing liquid, then rotation is evaporated to the 1/5 of standing liquid product at 45 DEG C, obtains concentrated gel liquid；It takes
Tantalum oxide is placed in ball grinder, the ball milling 3h under 250r/min, is crossed 200 mesh sieves and is obtained ball-milled powder, and then in mass ratio 1:15,
Ball-milled powder and concentrated gel liquid are stirred and are placed in ultrasonic disperse 10min under 200W, obtains modified dispersion liquid；By weight
It is white to weigh 55 parts of silicon rubber, 10 parts of modified dispersion liquids, 2 parts of Vulcanization accelerator TMTDs, 1 part of Cure of Rubber agent DBTU and 6 parts respectively for number meter
Carbon black is placed in open mill, is kneaded uniformly and is collected rubber compound, epoxy glue is placed under vulcanizing press, at 5MPa, 155 DEG C
Vulcanizing treatment 100min, standing are cooled to room temperature, you can are prepared into a kind of resistance to ablative insulative material of silicon rubber.
Example 2
In mass ratio 1：5, polyimide resin is added in n,N-dimethylacetamide, mixed liquor is obtained and is stirred, is dripped
N,N-dimethylacetamide dilution is added to handle, obtains dilution；In mass ratio 1:10, tantalic chloride is added in absolute ethyl alcohol, is stirred
It mixes and mixes to obtain lysate and by volume 1:10,5% glucose solution of mass fraction is added dropwise in lysate, control is added dropwise
Rate is 2mL/min, after being added dropwise to complete, is stirred and stands 27min and obtain modification liquid, counts, weigh respectively in parts by weight
47 parts of modification liquids, 12 parts of 1% aqueous povidone solutions of mass fraction and 2 parts of propylene oxide are placed in three-necked flask, are stirred
It mixes and mixes to obtain coagulant liquid, by volume 1:5, dilution is added in coagulant liquid, is stirred and is placed in water-bath at 57 DEG C and adds
Hot 11h after standing 44h, obtains standing liquid, then rotation is evaporated to the 1/5 of standing liquid product at 47 DEG C, obtains concentrated gel liquid；It takes
Tantalum oxide is placed in ball grinder, the ball milling 4h under 275r/min, is crossed 200 mesh sieves and is obtained ball-milled powder, and then in mass ratio 1:15,
Ball-milled powder and concentrated gel liquid are stirred and are placed in ultrasonic disperse 12min under 250W, obtains modified dispersion liquid；By weight
It is white to weigh 57 parts of silicon rubber, 12 parts of modified dispersion liquids, 2 parts of Vulcanization accelerator TMTDs, 2 parts of Cure of Rubber agent DBTU and 7 parts respectively for number meter
Carbon black is placed in open mill, is kneaded uniformly and is collected rubber compound, epoxy glue is placed under vulcanizing press, at 6MPa, 160 DEG C
Vulcanizing treatment 110min, standing are cooled to room temperature, you can are prepared into a kind of resistance to ablative insulative material of silicon rubber.
Example 3
In mass ratio 1：5, polyimide resin is added in n,N-dimethylacetamide, mixed liquor is obtained and is stirred, is dripped
N,N-dimethylacetamide dilution is added to handle, obtains dilution；In mass ratio 1:10, tantalic chloride is added in absolute ethyl alcohol, is stirred
It mixes and mixes to obtain lysate and by volume 1:10,5% glucose solution of mass fraction is added dropwise in lysate, control is added dropwise
Rate is 2mL/min, after being added dropwise to complete, is stirred and stands 30min and obtain modification liquid, counts, weigh respectively in parts by weight
50 parts of modification liquids, 15 parts of 1% aqueous povidone solutions of mass fraction and 2 parts of propylene oxide are placed in three-necked flask, are stirred
It mixes and mixes to obtain coagulant liquid, by volume 1:5, dilution is added in coagulant liquid, is stirred and is placed in water-bath at 65 DEG C and adds
Hot 12h after standing 48h, obtains standing liquid, then rotation is evaporated to the 1/5 of standing liquid product at 50 DEG C, obtains concentrated gel liquid；It takes
Tantalum oxide is placed in ball grinder, the ball milling 5h under 300r/min, is crossed 200 mesh sieves and is obtained ball-milled powder, and then in mass ratio 1:15,
Ball-milled powder and concentrated gel liquid are stirred and are placed in ultrasonic disperse 15min under 300W, obtains modified dispersion liquid；By weight
It is white to weigh 60 parts of silicon rubber, 15 parts of modified dispersion liquids, 3 parts of Vulcanization accelerator TMTDs, 2 parts of Cure of Rubber agent DBTU and 8 parts respectively for number meter
Carbon black is placed in open mill, is kneaded uniformly and is collected rubber compound, epoxy glue is placed under vulcanizing press, at 8MPa, 170 DEG C
Vulcanizing treatment 120min, standing are cooled to room temperature, you can are prepared into a kind of resistance to ablative insulative material of silicon rubber.
Example 1,2,3 prepared by the present invention carries out performance characterization, and specific test result is as shown in following table table 1：
The 1 performance table of comparisons of table
There is upper table to understand, heat-insulating material prepared by the present invention has excellent ablation resistance.
Claims (4)
1. a kind of preparation method of the resistance to ablative insulative material of silicon rubber, it is characterised in that specifically preparation process is：
（1）In mass ratio 1：5, polyimide resin is added in n,N-dimethylacetamide, mixed liquor is obtained and is stirred,
N,N-dimethylacetamide dilution processing is added dropwise, obtains dilution；
（2）In mass ratio 1:10, tantalic chloride is added in absolute ethyl alcohol, is stirred to obtain lysate and by volume 1:10,
Glucose solution is added dropwise in lysate, after being added dropwise to complete, is stirred and stands, obtain modification liquid；
（3）It counts in parts by weight, weighs 45~50 parts of modification liquids, 10~15 parts of aqueous povidone solutions and 1~2 respectively
Part propylene oxide is placed in three-necked flask, is stirred to obtain coagulant liquid, and by volume 1:5, dilution is added in coagulant liquid,
Simultaneously heating water bath is stirred, after standing 40~48h, obtains standing liquid；
（4）Liquid rotary evaporation will be stood, concentrated gel liquid is obtained, tantalum oxide is taken to be placed in ball grinder, ball milling sieves to obtain ball milling powder
End, then in mass ratio 1:15, ball-milled powder and concentrated gel liquid are stirred simultaneously ultrasonic disperse, obtain modified dispersion liquid；
（5）It counts in parts by weight, weighs 55~60 parts of silicon rubber, 10~15 parts of modified dispersion liquids, 2~3 parts of rush respectively through agent
TMTD, 1~2 part of Cure of Rubber agent DBTU and 6~8 parts of white carbons are placed in open mill, are kneaded uniformly and are collected rubber compound, will be mixed
Rubber alloy is placed under vulcanizing press, and vulcanizing treatment, standing is cooled to room temperature, you can is prepared into a kind of silicon rubber heat insulating material of resistance to ablation
Material.
2. a kind of preparation method of the resistance to ablative insulative material of silicon rubber according to claim 1, it is characterised in that：Step
（2）The glucose solution drop rate is 2mL/min.
3. a kind of preparation method of the resistance to ablative insulative material of silicon rubber according to claim 1, it is characterised in that：Step
（4）The rotating evaporation temperature is 45~50 DEG C.
4. a kind of preparation method of the resistance to ablative insulative material of silicon rubber according to claim 1, it is characterised in that：Step
（5）The vulcanizing treatment condition is in 5~8MPa, 155~170 DEG C of vulcanizing treatments.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110079091A (en) * | 2019-03-25 | 2019-08-02 | 常州达奥新材料科技有限公司 | A kind of preparation method of resistance to ablation composite insulation material |
| CN110346400A (en) * | 2019-06-18 | 2019-10-18 | 北京科技大学 | A kind of experimental rig and method for simulating Cannon burning |
| CN111392726A (en) * | 2020-03-09 | 2020-07-10 | 西安理工大学 | Method for preparing TaC organic precursor and nano-particles thereof by rotary evaporation |
-
2017
- 2017-12-30 CN CN201711488208.2A patent/CN108084714A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110079091A (en) * | 2019-03-25 | 2019-08-02 | 常州达奥新材料科技有限公司 | A kind of preparation method of resistance to ablation composite insulation material |
| CN110346400A (en) * | 2019-06-18 | 2019-10-18 | 北京科技大学 | A kind of experimental rig and method for simulating Cannon burning |
| CN111392726A (en) * | 2020-03-09 | 2020-07-10 | 西安理工大学 | Method for preparing TaC organic precursor and nano-particles thereof by rotary evaporation |
| CN111392726B (en) * | 2020-03-09 | 2023-01-24 | 西安理工大学 | Method for preparing TaC organic precursor and nano-particles thereof by rotary evaporation |
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