CN102643547A - Ablation-resistant room temperature vulcanized silicone rubber and preparation method thereof - Google Patents
Ablation-resistant room temperature vulcanized silicone rubber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an ablation-resistant room temperature vulcanized silicone rubber which comprises the components in parts by weight: 94-99 parts of base glue, 1-5 parts of flame retardant auxiliary agent, 0.3-0.6 part of vulcanization accelerator and 0.05-0.1 part of auxiliary agent. The ablation-resistant room temperature vulcanized silicone rubber is good in physical and mechanical properties, and the requirements of a molding construction technology can be met by the operation performance.
Description
Technical field
The present invention relates to room temperature vulcanized silicone rubber, particularly relate to a kind of room temperature vulcanized liquid silicone rubber of anti-ablation the and working method thereof.
Background technology
The ordinary silicon rubber packing material can use under 250~300 ℃ condition.But when using as the coating material of anti-the ablation, its performance just is difficult to satisfy request for utilization.Zhong Hao Chenguang Research Institute of Chemical Industry is employed in the phase at the beginning of the eighties in last century and adds high thermal resistance and the flame retardant resistance that a large amount of fire retardant material methods improve Zylox in the room temperature vulcanized silicone rubber, can make the thermotolerance of Zylox bring up to 500~800 ℃; We have begun to introduce phenyl in the beginning of this century and the sample collected recently and Muscovite pertinent data introduction but still will adopt the mode that adds fire-retardant filler to realize improving the Zylox ablation resistance, to such an extent as to but these methods all can cause the flowability of Zylox to descend significantly is difficult to use in the occasion that the perfusion form is used.
Summary of the invention
The purpose of this invention is to provide a kind of room temperature vulcanized silicone rubber of anti-the ablation, this product should have preferably ablation resistance and have higher physical and mechanical properties simultaneously and can satisfy user's perfusion needs in use.
The present invention provides a kind of room temperature vulcanized silicone rubber of anti-the ablation, and it is processed by following component by weight ratio:
Basis glue 94~99
Flame retardant 1~5
Vulcanization accelerator 0.3~0.6
Auxiliary agent 0.05~0.1.
The room temperature vulcanized silicone rubber of anti-ablation the of the present invention; Wherein said basic glue main chain is by gathering the phenylbenzene dimethyl siloxane, gathering one or more oligomers in ethylene methacrylic radical siloxane and the YSR 3286; Make with the organosilicon hydrolyzation thing that contains one or more groups in methyl, vinyl and the phenyl (the commercially available acquisition of raw material for preparing this hydrolyzate) copolymerization; Gained multipolymer viscosity is at 6000mPas~16000mPas, preferred 8000mPas~16000mPas, and end group is a hydroxyl.
Wherein, the viscosity of said oligomer is 12mPas~50mPas; The viscosity of said organosilicon hydrolyzation thing is 3.5mPas~35mPas.
The said organosilicon hydrolyzation thing that contains one or more groups in methyl, vinyl and the phenyl is prepared by following method: the Ethoxysilane that will contain one or more groups in methyl, vinyl and the phenyl; Under trace acid and certain temperature condition; Carry out quantitative hydrolysis reaction; With the organic bases neutralization, remove low molecule more then, filtration promptly gets.
Said flame retardant by contain Pt compound (can commercially availablely obtain) and organosilicon oligopolymer carry out complexing again with contain phenyl, methyl and vinyl in the ZGK 5 of one or more groups mix and remove low molecule and make.
For example, contain Pt compound such as Platinic chloride, under 80 ℃~160 ℃ condition, reacted 2~4 hours with divinyl tetramethyl disiloxane; Be washed till neutrality with deionized water, after dry 24 hours, join and gather in the phenylbenzene dimethyl siloxane; Remove volatile matter, get the mixture of an anti-flaming transparent.
Said vulcanization accelerator is selected from positive silicic acid tin, one or more in stannous octoate and the dibutyl tin laurate.
Said auxiliary agent is selected from one or more in hydroxy silicon oil, YSR 3286, hydroxyl breast and the deionized water, and when auxiliary agent was non-deionized water, viscosity was 10mPas~30mPas.
The present invention also provides the preparation method of the said room temperature vulcanized silicone rubber of anti-the ablation: the basic glue with formula ratio adds in the conversion unit earlier, and in 50~100 ℃, stirring velocity is 120~300 rev/mins; Under the condition of overbottom pressure 0.085Mpa; Kept 60~90 minutes, and be cooled to 60 ℃, add flame retardant, the auxiliary agent of formula ratio; Kept 60~90 minutes, and filtered discharging as the A component; Vulcanization accelerator is as the B component.During use, the B component added in the A component row's of stirring bubble in proportion after, can pour into.
The performance index of the room temperature vulcanized silicone rubber of anti-ablation the according to the invention are as shown in table 1 below:
Table 1
The present invention has following beneficial effect:
Adopt suitable operational path and prescription, overcome the deficiency in the like product production technology, a kind of room temperature vulcanized silicone rubber of anti-the ablation is provided, its physical and mechanical properties is good, and processing property satisfies the in-place mo(u)lding construction process requirement.
Embodiment
Following examples are used to explain the present invention, but are not used for limiting scope of the present invention.
Each component is available from Zhong Hao Chenguang Research Institute of Chemical Industry or be the commercial goods in the present invention prescription.
Fill a prescription used concrete component and manufacturer of the present invention is following:
Platinic chloride, Shenyang gold section chemical industry;
The vinyl cyclotetrasiloxane, Zhong Hao Chenguang Research Institute of Chemical Industry organosilicon factory;
Octamethylcyclotetrasiloxane, Zhong Hao Chenguang Research Institute of Chemical Industry organosilicon factory;
The benzyl ring tetrasiloxane, Zhong Hao Chenguang Research Institute of Chemical Industry organosilicon factory;
Union carbide A-162, Zhong Hao Chenguang Research Institute of Chemical Industry organosilicon factory;
Phenyl triethoxysilane, Zhong Hao Chenguang Research Institute of Chemical Industry organosilicon factory;
Vinyltriethoxysilane, Zhong Hao Chenguang Research Institute of Chemical Industry organosilicon factory;
Embodiment 1
1) preparation of organosilicon hydrolyzation thing:
Vinyltriethoxysilane 50kg is put in the lass lining conversion unit that has TM and stirring and dropping mouth, open and stir, add micro-hydrochloric acid; Be warmed up to 80 ℃, drip deionized water, after reaction finishes; Neutralize with hexamethyldisilazane; Filter, remove low molecule again, getting viscosity is the organosilicon hydrolyzation thing that contains vinyl of 16mPas.
2) preparation of basic glue:
In the polymerizer that has devices such as stirring, TM, heating, vacuum system; Add octamethylcyclotetrasiloxane 100kg and dimethyldiethoxysilane 25kg; Under the effect of catalyzer TMAH alkali glue 0.15kg; Reacted 5 hours down in 115 ℃, in equipment, remove low molecule then and make balance silicone oil.Again balance silicone oil 100kg is moved in the glass lined reaction vessel that has heating unit; Add toluene 60kg and hydrochloric acid (concentration is 36.5wt%) 0.5kg, reaction is 4 hours under the refluxing toluene temperature, is cooled to room temperature water and is washed till neutrality; Standing demix; Branch vibration layer removes solvent and low molecule, makes the organosilicon oligomer that viscosity is the YSR 3286 of hydroxyl for the 20mPas end group.
In the polycondensation reactor that has heating and vacuum unit; Add above-mentioned oligomer 65kg, organosilicon hydrolyzation thing 35kg and 60kg YLENE; Zinc octoate 0.03kg carries out polycondensation under the refluxing xylene temperature, the low molecule that in reaction, removes reaches 2kg; Decompression removes YLENE and low molecule again, viscosity is that the end group of 8500mPas is the basic glue of hydroxyl.
3) preparation of platiniferous phenyl silicone oil:
Platinic chloride 0.04kg and the stirring of divinyl tetramethyl disiloxane 2kg adding band, temperature are taken into account in the there-necked flask of reflux; Reaction is 2 hours under 120 ℃ condition; Be washed till neutrality with deionized water, after dry 24 hours, be filled into and gather among the phenylbenzene dimethyl siloxane 20kg; Remove volatile matter, get brown transparent platiniferous phenyl silicone oil.
4) preparation of the room temperature vulcanized silicone rubber of anti-ablation A component:
Basic glue 96KG adding is had in the equipment of stirring and heating and vacuum system, and regulating mixing speed is 120 rev/mins, is warming up to 100 ℃, the open vacuum pump; Overbottom pressure 0.085Mpa kept 60 minutes, was cooled to 60 ℃ then, added platiniferous phenyl silicone oil 4KG and hydroxy silicon oil 0.05KG; Kept 1 hour, cooling through 120 order filtering nets, filters and packages; Getting basic glue is A component 98KG, and its viscosity is for being 11000mPas, and end group is a hydroxyl;
With the positive silicic acid tin of 0.3KG pack the B component.
5) method of use of the present invention's room temperature vulcanized silicone rubber of anti-the ablation is:
Behind the row's of stirring bubble in the B component adding A component, can pour into.
The room temperature vulcanized silicone rubber of anti-ablation that the present invention makes is as shown in table 2 with the similar rubber performance of the method preparation of introducing by foreign literature.
Table 2
Show by table 2 performance comparison, the present invention's room temperature vulcanized silicone rubber of anti-the ablation, ablation resistance is suitable with external sample, and mobile, physicals is superior to external sample, and liquid silastic in-place mo(u)lding property and good physical and mechanical properties obtain embodying.Can be used as military project powder charge coating material and powder charge immobilization material.
Embodiment 2
1) preparation of organosilicon hydrolyzation thing:
Union carbide A-162 50kg is put in the lass lining conversion unit that has TM and stirring and dropping mouth, open and stir, add micro-hydrochloric acid; Be warmed up to 80 ℃; Drip deionized water, after reaction finishes, neutralize with sodium ethylate; Remove low molecule again, getting viscosity is the methylic organosilicon hydrolyzation thing of 12mPas.
2) preparation of basic glue:
85kg octamethylcyclotetrasiloxane, 15kg tetramethyl-tetrem alkenyl siloxane and dimethyldiethoxysilane 25kg are joined in the polymerizer of devices such as having stirring, TM, heating, vacuum; Under the effect of catalyzer TMAH alkali glue 0.14kg; Reacted 5 hours down in 115 ℃, in equipment, remove low molecule then and make balance silicone oil.Again balance silicone oil 100kg is moved in the glass lined reaction vessel that has heating unit; Adding toluene 60kg and hydrochloric acid (concentration is 36.5wt%) 0.5kg reacted 4 hours under the refluxing toluene temperature; Be cooled to room temperature water and be washed till neutrality, standing demix, branch vibration layer; Remove solvent and low molecule, making viscosity is the YSR 3286 and the organosilicon oligomer that gathers the ethylene methacrylic radical siloxane of hydroxyl for the 24mPas end group.
In the polycondensation reactor that has heating and vacuum unit; Add above-mentioned oligomer 55kg, organosilicon hydrolyzation thing 45 and 60kg YLENE; Zinc octoate 0.03kg carries out polycondensation under the refluxing xylene temperature, the low molecule that in reaction, removes reaches 1kg; Decompression removes YLENE and low molecule again, viscosity is that the end group of 8700mPas is the basic glue of hydroxyl.
3) preparation of platiniferous polymethyl siloxane:
Platinic chloride 0.04kg and the stirring of divinyl tetramethyl disiloxane 2kg adding band, temperature are taken into account in the there-necked flask of reflux; Reaction is 2 hours under 120 ℃ condition; Be washed till neutrality with deionized water, after dry 24 hours, be filled among the YSR 3286 20kg; Remove volatile matter, get faint yellow transparent platiniferous methylsiloxane.
4) preparation of the room temperature vulcanized silicone rubber of anti-ablation A component, B component:
With basic glue 95KG, adding has in the equipment of stirring and heating and vacuum system, and regulating mixing speed is 300 rev/mins, is warming up to 100 ℃; The open vacuum pump, overbottom pressure 0.085Mpa kept 90 minutes, was cooled to 60 ℃ then; Add platiniferous polymethyl siloxane 5KG and auxiliary agent 0.1KG hydroxy silicon oil, kept 60 minutes, cooling is through 120 order filtering nets; Filter and package, get A component 98.5KG, its viscosity is 12000mPas, and end group is a hydroxyl; With positive silicic acid tin 0.6KG pack the B component.
During use, behind the row's of stirring bubble in the B component adding A component, can pour into.Its test piece performance such as following table.
Table 3
Embodiment 3
1) preparation of organosilicon hydrolyzation thing:
Union carbide A-162 and vinyltriethoxysilane (7: 3 in molar ratio ratios) are put in the lass lining conversion unit that has TM and stirring and dropping mouth, opened and stir, add micro-hydrochloric acid; Be warmed up to 80 ℃; Drip deionized water, after reaction finishes, neutralize with sodium ethylate; Remove low molecule again, getting viscosity is the methyl ethylene organosilicon hydrolyzation thing of 15mPas.
2) preparation of basic glue:
75kg octamethylcyclotetrasiloxane and 25kg octaphenyl cyclotetrasiloxane and 25kg dimethyldiethoxysilane are joined in the polymerizer of devices such as having stirring, TM, heating, vacuum; Under the effect of 0.2kg TMAH alkali glue; Reacted 5 hours down in 125 ℃, in equipment, remove low molecule then and make balance silicone oil.Again balance silicone oil 100kg is moved in the glass lined reaction vessel that has heating unit; Add toluene 60kg and catalyzer hydrochloric acid (concentration is 36.5wt%) 0.5kg, reaction is 4 hours under the refluxing toluene temperature, is cooled to room temperature water and is washed till neutrality; Standing demix; Branch vibration layer removes solvent and low molecule, and making viscosity is the oligomer of hydroxyl for the 25mPas end group.
In the polycondensation reactor that has heating and vacuum unit; Add above-mentioned oligomer 50kg, organosilicon hydrolyzation thing 50kg and YLENE 60kg, zinc octoate 0.03kg carries out polycondensation under the refluxing xylene temperature; The low molecule that in reaction, removes reaches 0.8kg; Decompression removes low molecule again, and getting viscosity is 10000mPas, and end group is the basic glue that contains methyl, phenyl and vinyl of hydroxyl.
3) platiniferous gathers the preparation of ethylene methacrylic radical siloxane:
Platinic chloride 04kg and the stirring of divinyl tetramethyl disiloxane 2kg adding band, temperature are taken into account in the there-necked flask of reflux; Reaction is 2 hours under 120 ℃ condition; Be washed till neutrality with deionized water, after dry 24 hours, be filled into and gather among the ethylene methacrylic radical siloxane 20kg; Remove volatile matter, get faint yellow transparent platiniferous ethylene methacrylic radical siloxane.
4) preparation of the room temperature vulcanized silicone rubber of anti-ablation A component, B component:
Basic glue 98.5kg adding is had in the equipment of stirring and heating and vacuum system, and regulating mixing speed is 120 rev/mins, is warming up to 100 ℃, the open vacuum pump; Overbottom pressure 0.085Mpa kept 90 minutes, was cooled to 60 ℃ then, added platiniferous and gathered ethylene methacrylic radical siloxane 1.5kg and hydroxyl breast 0.1kg; Kept 60 minutes, cooling through 120 order filtering nets, filters and packages; Get A component 99kg, its viscosity is at 13000mPas, and end group is a hydroxyl;
With dibutyl tin laurate (0.3kg) packing, get the B component.
During use, behind the row's of stirring bubble in the B component adding A component, can pour into.Make test piece performance such as following table by this.
Table 4
Embodiment 4
1) preparation of organosilicon hydrolyzation thing:
Union carbide A-162, vinyltriethoxysilane, phenyl triethoxysilane were put in the lass lining conversion unit that has TM and stirring and dropping mouth in 92: 3: 5 in molar ratio, opened and stir, add micro-hydrochloric acid; Be warmed up to 80 ℃; Drip deionized water, after reaction finishes, with the sodium ethylate neutrality that neutralizes; Remove low molecule, getting viscosity is the organosilicon hydrolyzation thing that contains methyl, vinyl and phenyl of 17mPas.
2) preparation of basic glue:
65kg octamethylcyclotetrasiloxane, 25kg octaphenyl cyclotetrasiloxane and 10kg tetramethyl-tetrem thiazolinyl cyclotetrasiloxane and dimethyldiethoxysilane 25kg are joined in the polymerizer of devices such as having stirring, TM, heating, vacuum; Under the effect of 0.25kg catalyzer TMAH alkali glue; Reacted 5 hours down in 120 ℃, in equipment, remove low molecule then and make balance silicone oil.Again balance silicone oil 100kg is moved in the glass lined reaction vessel that has heating unit; Add toluene 60kg and 0.5kg hydrochloric acid (concentration is 36.5wt%), reaction is 4 hours under the refluxing toluene temperature, is cooled to room temperature water and is washed till neutrality; Standing demix; Branch vibration layer removes solvent and low molecule, and the viscosity that makes the end group that contains phenyl, vinyl and be hydroxyl is 30mPas organosilicon oligomer.
In the polycondensation reactor that has heating and vacuum unit; Add above-mentioned oligomer 50kg, organosilicon hydrolyzation thing 50kg and YLENE 60kg, octoate catalyst tin 0.03kg carries out polycondensation under the refluxing xylene temperature; The low molecule that in reaction, removes reaches 0.75kg; Decompression removes YLENE and low molecule again, and getting viscosity is 14000mPas, and end group is the basic glue that contains phenyl and vinyl of hydroxyl.
3) preparation of platiniferous methyl-silicone oil:
Platinic chloride 0.4kg and the stirring of divinyl tetramethyl disiloxane 2kg adding band, temperature are taken into account in the there-necked flask of reflux; Reaction is 2 hours under 120 ℃ condition; Be washed till neutrality with deionized water, after dry 24 hours, be filled among the YSR 3286 20kg; Remove volatile matter, get faint yellow transparent platiniferous methylsiloxane.
4) preparation of the room temperature vulcanized silicone rubber of anti-ablation A component, B component:
Basic glue 99kg adding is had in the equipment of stirring and heating and vacuum system, and regulating mixing speed is 200 rev/mins, is warming up to 100 ℃, the open vacuum pump; Overbottom pressure 0.085Mpa kept 60~90 minutes, was cooled to 60 ℃ then, added platiniferous methyl-silicone oil 1kg and deionized water 0.1kg; Kept 1 hour, cooling through 120 order filtering nets, filters and packages; Get A component 99kg, end group is a hydroxyl, and viscosity is 15800mPas.
With stannous octoate (0.3kg) packing, get the B component.
During use, behind the row's of stirring bubble in the B component adding A component, can pour into.It is as shown in the table to make the test piece performance.
Table 5
Embodiment 5
1) preparation of organosilicon hydrolyzation thing:
Union carbide A-162 and vinyltriethoxysilane (8: 2 in molar ratio ratios) are put in the lass lining conversion unit that has TM and stirring and dropping mouth, opened and stir, add micro-hydrochloric acid; Be warmed up to 80 ℃; Drip deionized water, after reaction finishes, be neutralized to neutrality with sodium ethylate; Remove low molecule, getting viscosity is the organosilicon hydrolyzation thing that contains methyl and vinyl of 14mPas.
2) preparation of basic glue:
In the polymerizer that has devices such as stirring, TM, heating, vacuum; Add octamethylcyclotetrasiloxane 100kg and dimethyldiethoxysilane 25kg; Under the effect of catalyzer TMAH 0.2kg; Reacted 5 hours down in 110 ℃, in equipment, remove low molecule then and make balance silicone oil.Again balance silicone oil 100kg is moved in the glass lined reaction vessel that has heating unit; Add toluene 60kg and catalyzer hydrochloric acid (concentration is 36.5wt%) 0.5kg, reaction is 4 hours under the refluxing toluene temperature, is cooled to room temperature water and is washed till neutrality; Standing demix; Branch vibration layer removes YLENE and low molecule, and making viscosity is the organosilicon oligomer of hydroxyl for the 16mPas end group.
In the polycondensation reactor that has heating and vacuum unit; Add above-mentioned oligomer 70KG, organosilicon hydrolyzation thing 30KG and YLENE 60kg; Octoate catalyst zinc 0.03kg carries out polycondensation under the refluxing xylene temperature, the low molecule that in reaction, removes reaches 0.75kg; Decompression removes low molecule again, and getting viscosity is the basic glue of hydroxyl for the 6300mPas end group.
3) preparation of platiniferous phenyl silicone oil:
Platinic chloride 0.04kg and the stirring of divinyl tetramethyl disiloxane 2kg adding band, temperature are taken into account in the there-necked flask of reflux; Reaction is 2 hours under 120 ℃ condition; Be washed till neutrality with deionized water, after dry 24 hours, be filled into and gather among the phenylbenzene dimethyl siloxane 2kg; Remove volatile matter, get brown transparent platiniferous phenyl silicone oil.
4) preparation of the present invention's room temperature vulcanized silicone rubber of anti-ablation A component, B component:
Basic glue 97kg adding is had in the equipment of stirring and heating and vacuum system, and regulating mixing speed is 180 rev/mins, is warming up to 100 ℃, the open vacuum pump; Overbottom pressure 0.085Mpa kept 3 hours, was cooled to 60 ℃ then, added platiniferous phenyl silicone oil 3kg and hydroxy silicon oil 0.1kg; Kept 1 hour, cooling is through 120 order filtering nets; Filter and package, get A component 99kg, viscosity is 8300mPas;
With stannous octoate 0.5kg packing, get the B component.
During use, behind the row's of stirring bubble in the B component adding A component, can pour into.This test piece performance such as following table.
Table 6
Claims (8)
1. the room temperature vulcanized silicone rubber of anti-the ablation is characterized in that, is processed by following components by part by weight:
94~99 parts in basis glue
1~5 part of flame retardant
0.3~0.6 part of vulcanization accelerator
0.05~0.1 part of auxiliary agent.
2. the room temperature vulcanized silicone rubber of anti-ablation the as claimed in claim 1; It is characterized in that; One or more oligomers that said basic glue main chain gathers the phenylbenzene dimethyl siloxane by being selected from, gather in ethylene methacrylic radical siloxane and the YSR 3286 make with the organosilicon hydrolyzation thing copolymerization that contains one or more groups in methyl, vinyl and the phenyl; Gained multipolymer viscosity is between 6000mPas~16000mPas, and end group is a hydroxyl.
3. the room temperature vulcanized silicone rubber of anti-ablation the as claimed in claim 2 is characterized in that, the viscosity of said oligomer is 12mPas~50mPas.
4. the room temperature vulcanized silicone rubber of anti-ablation the as claimed in claim 2; It is characterized in that the said organosilicon hydrolyzation thing that contains one or more groups in methyl, vinyl and the phenyl is prepared by following method: will contain the Ethoxysilane of one or more groups in methyl, vinyl and the phenyl, under trace acid and certain temperature condition; Carry out quantitative hydrolysis reaction; With the organic bases neutralization, remove low molecule more then, filtration promptly gets; The viscosity of gained organosilicon hydrolyzation thing is 3.5mPas~35mPas.
5. the room temperature vulcanized silicone rubber of anti-ablation the as claimed in claim 1; It is characterized in that, said flame retardant by contain platinic compound and organosilicon oligopolymer carry out complexing again with contain phenyl, methyl or vinyl in the ZGK 5 of one or more groups mix and remove low molecule and make.
6. the room temperature vulcanized silicone rubber of anti-ablation the as claimed in claim 1 is characterized in that, said vulcanization accelerator is selected from one or more in positive silicic acid tin, stannous octoate and the dibutyl tin laurate.
7. the room temperature vulcanized silicone rubber of anti-ablation the as claimed in claim 1 is characterized in that, said auxiliary agent is selected from one or more in hydroxy silicon oil, YSR 3286, hydroxyl breast and the deionized water.
8. prepare the method for the described room temperature vulcanized silicone rubber of anti-ablation of claim 1, it is characterized in that, in the basic glue adding conversion unit with formula ratio; In 50~100 ℃, stirring velocity is 120~300 rev/mins, under the condition of overbottom pressure 0.085Mpa; Kept 60~90 minutes, and be cooled to 60 ℃, add flame retardant, the auxiliary agent of formula ratio; Kept 60~90 minutes, and filtered discharging as the A component; Vulcanization accelerator, behind the row's of stirring bubble in the B component adding A component, can pour into during use as the B component.
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CN105669980B (en) * | 2016-02-17 | 2018-08-28 | 合肥工业大学 | A kind of alpha, omega end vinyl silicone oil of phenyl-fluoride hydrocarbon backbone boracic and preparation method thereof |
CN109852238A (en) * | 2019-01-09 | 2019-06-07 | 上海交通大学 | A kind of sprayable resistance to ablative coatings of silicon rubber base lightweight and its application |
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 |
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