CN102643547B - 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 production method thereof.
Background technology
The ordinary silicon rubber packing material can be used under the condition of 250～300 ℃.But, when using as the coating material of anti-the ablation, its performance just is difficult to meet service requirements.Zhong Hao Chenguang Research Institute of Chemical Industry adopted and in room temperature vulcanized silicone rubber, adds a large amount of fire retardant material methods to improve high thermal resistance and the flame retardant resistance of silicon rubber in the phase at the beginning of the eighties in last century, can make the thermotolerance of silicon rubber bring up to 500～800 ℃; We have started 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 silicon rubber ablation resistance, to such an extent as to but these methods all can cause the mobility of silicon rubber significantly to descend 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 ablation resistance preferably and have higher physical and mechanical properties simultaneously and can meet user's perfusion needs in use.
The invention provides a kind of room temperature vulcanized silicone rubber of anti-the ablation, it is made 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 one or more oligomers in poly-phenylbenzene dimethyl siloxane, poly-ethylene methacrylic radical siloxane and polydimethylsiloxane, with organosilicon hydrolyzation thing (the commercially available acquisition of raw material for preparing this hydrolyzate) copolymerization that contains one or more groups in methyl, vinyl and phenyl, make, gained multipolymer viscosity is at 6000mPas～16000mPas, preferred 8000mPas～16000mPas, end group is hydroxyl.
Wherein, the viscosity of described oligomer is 12mPas～50mPas; The viscosity of described organosilicon hydrolyzation thing is 3.5mPas～35mPas.
Prepared by following method by the described organosilicon hydrolyzation thing containing one or more groups in methyl, vinyl and phenyl: the Ethoxysilane that will contain one or more groups in methyl, vinyl and phenyl, under Determining Micro Acid and certain temperature condition, carry out quantitative hydrolysis reaction, then with organic bases, neutralize, remove again low molecule, filter and get final product.
Described flame retardant mixes with the polysiloxane of one or more groups containing in phenyl, methyl and vinyl to remove again and hangs down molecule and make by carry out complexing containing Pt compound (being commercially available) and silicone oligomer.
For example, containing the Pt compound, as Platinic chloride, with divinyl tetramethyl disiloxane, under the condition of 80 ℃～160 ℃, react 2～4 hours, be washed till neutrality with deionized water, after dry 24 hours, join in poly-phenylbenzene dimethyl siloxane, remove volatile matter, obtain the mixture of an anti-flaming transparent.
Described vulcanization accelerator is selected from positive silicic acid tin, one or more in stannous octoate and dibutyl tin laurate.
Described auxiliary agent is selected from one or more in hydroxy silicon oil, polydimethylsiloxane, hydroxyl breast and deionized water, and when auxiliary agent is non-deionized water, viscosity is 10mPas～30mPas.
The present invention also provides the preparation method of the described room temperature vulcanized silicone rubber of anti-the ablation: first the basic glue of formula ratio is added in conversion unit, in 50～100 ℃, stirring velocity is 120～300 rev/mins, under the condition of overbottom pressure 0.085Mpa, maintain 60～90 minutes, be cooled to 60 ℃, add flame retardant, the auxiliary agent of formula ratio, maintain 60～90 minutes, filter discharging as the A component; Vulcanization accelerator is as the B component.During use, after the B component is added in the A component to the row's of stirring evenly bubble in proportion, can pour into.
The performance index of the room temperature vulcanized silicone rubber of anti-ablation the of the present invention are as shown in table 1 below:
Table 1
The present invention has following beneficial effect:
Adopt suitable operational path and formula, 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 meets the in-place mo(u)lding construction process requirement.
Embodiment
Following examples are used for the present invention is described, but are not used for limiting the scope of the invention.
In the present invention formula, each component is purchased from Zhong Hao Chenguang Research Institute of Chemical Industry or be commercial goods.
The present invention fill a prescription concrete component used and manufacturer as follows:
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 into thermometer and stirring and drips in the lass lining conversion unit of mouth, open and stir, add micro-hydrochloric acid, be warmed up to 80 ℃, drip deionized water, when after completion of the reaction, with hexamethyldisilazane, neutralize, filter, then remove low molecule, obtaining viscosity is the organosilicon hydrolyzation thing containing vinyl of 16mPas.
2) preparation of basic glue:
In the polymerizer with devices such as stirring, thermometer, heating, vacuum systems, add octamethylcyclotetrasiloxane 100kg and dimethyldiethoxysilane 25kg, under the effect of catalyzer Tetramethylammonium hydroxide alkali glue 0.15kg, under 115 ℃, reaction is 5 hours, then in same equipment, removes low molecule and makes balance silicone oil.Again balance silicone oil 100kg is moved in the glass lined reaction vessel with heating unit, add toluene 60kg and hydrochloric acid (concentration is 36.5wt%) 0.5kg, at the refluxing toluene temperature, reaction is 4 hours, be cooled to room temperature water and be washed till neutrality, stratification, branch vibration layer, desolvation and low molecule, the organosilicon oligomer of the polydimethylsiloxane that to make viscosity and be the 20mPas end group be hydroxyl.
In the polycondensation reactor with heating and vacuum unit, add above-mentioned oligomer 65kg, organosilicon hydrolyzation thing 35kg and 60kg dimethylbenzene, zinc octoate 0.03kg, carry out polycondensation at the refluxing xylene temperature, the low molecule removed in reaction reaches 2kg, decompression removes dimethylbenzene and low molecule again, the basic glue that the end group that to obtain viscosity be 8500mPas is hydroxyl.
3) preparation of platiniferous phenyl silicone oil:
Add band stirring, temperature to take into account in the there-necked flask of reflux Platinic chloride 0.04kg and divinyl tetramethyl disiloxane 2kg, under the condition of 120 ℃, reaction is 2 hours, be washed till neutrality with deionized water, after dry 24 hours, be filled in poly-phenylbenzene dimethyl siloxane 20kg, remove volatile matter, obtain brown transparent platiniferous phenyl silicone oil.
4) preparation of the room temperature vulcanized silicone rubber of anti-ablation A component:
Basic glue 96KG is added in the equipment with stirring and heating and vacuum system, and regulating mixing speed is 120 rev/mins, is warming up to 100 ℃, open vacuum pump, overbottom pressure 0.085Mpa, maintain 60 minutes, then be cooled to 60 ℃, add platiniferous phenyl silicone oil 4KG and hydroxy silicon oil 0.05KG, maintain 1 hour, cooling, through 120 order filtering nets, filter and package, obtaining basic glue is A component 98KG, its viscosity is for being 11000mPas, and end group is hydroxyl;
The positive silicic acid tin of 0.3KG is packed to obtain to the B component.
5) using method of the present invention's room temperature vulcanized silicone rubber of anti-the ablation is:
After the B component is added in the A component to the row's of stirring evenly bubble, can pour into.
Similar rubber performance prepared with method by the foreign literature introduction by the room temperature vulcanized silicone rubber of anti-ablation that the present invention makes is compared as shown in table 2.
Table 2
By table 2 performance comparison, shown, the present invention's room temperature vulcanized silicone rubber of anti-the ablation, ablation resistance and abroad are suitable, and mobility, physicals are better than abroad, and liquid silastic in-place mo(u)lding and good physical and mechanical properties are embodied.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 into thermometer and stirring and drips in the lass lining conversion unit of mouth, open and stir, add micro-hydrochloric acid, be warmed up to 80 ℃, drip deionized water, when after completion of the reaction, neutralize with sodium ethylate, remove low molecule, obtaining viscosity is the methylic organosilicon hydrolyzation thing of 12mPas again.
2) preparation of basic glue:
85kg octamethylcyclotetrasiloxane, 15kg tetramethyl-tetrem alkenyl siloxane and dimethyldiethoxysilane 25kg are joined in the polymerizer with devices such as stirring, thermometer, heating, vacuum, under the effect of catalyzer Tetramethylammonium hydroxide alkali glue 0.14kg, under 115 ℃, reaction is 5 hours, then in same equipment, removes low molecule and makes balance silicone oil.Again balance silicone oil 100kg is moved in the glass lined reaction vessel with heating unit, add toluene 60kg and hydrochloric acid (concentration is 36.5wt%) 0.5kg to react 4 hours at the refluxing toluene temperature, be cooled to room temperature water and be washed till neutrality, stratification, branch vibration layer, desolvation and low molecule, the polydimethylsiloxane that to make viscosity and be the 24mPas end group be hydroxyl and the organosilicon oligomer of poly-ethylene methacrylic radical siloxane.
In the polycondensation reactor with heating and vacuum unit, add above-mentioned oligomer 55kg, organosilicon hydrolyzation thing 45 and 60kg dimethylbenzene, zinc octoate 0.03kg, carry out polycondensation at the refluxing xylene temperature, the low molecule removed in reaction reaches 1kg, decompression removes dimethylbenzene and low molecule again, the basic glue that the end group that to obtain viscosity be 8700mPas is hydroxyl.
3) preparation of platiniferous polymethyl siloxane:
Add band stirring, temperature to take into account in the there-necked flask of reflux Platinic chloride 0.04kg and divinyl tetramethyl disiloxane 2kg, under the condition of 120 ℃, reaction is 2 hours, be washed till neutrality with deionized water, after dry 24 hours, be filled in polydimethylsiloxane 20kg, remove volatile matter, obtain faint yellow transparent platiniferous methylsiloxane.
4) preparation of the room temperature vulcanized silicone rubber of anti-ablation A component, B component:
By basic glue 95KG, add in the equipment with stirring and heating and vacuum system, regulating mixing speed is 300 rev/mins, be warming up to 100 ℃, open vacuum pump, overbottom pressure 0.085Mpa, maintain 90 minutes, then be cooled to 60 ℃, add platiniferous polymethyl siloxane 5KG and auxiliary agent 0.1KG hydroxy silicon oil, maintain 60 minutes, cooling, through 120 order filtering nets, filter and package, obtain A component 98.5KG, its viscosity is 12000mPas, and end group is hydroxyl; Positive silicic acid tin 0.6KG is packed to obtain to the B component.
During use, after the B component is added in the A component to the row's of stirring evenly bubble, can pour into.Its test piece performance is as following table.
Table 3
Embodiment 3
1) preparation of organosilicon hydrolyzation thing:
Union carbide A-162 and vinyltriethoxysilane (ratios of 7: 3 in molar ratio) are put into thermometer and stirring and dripped in the lass lining conversion unit of mouth, open and stir, add micro-hydrochloric acid, be warmed up to 80 ℃, drip deionized water, when after completion of the reaction, neutralize with sodium ethylate, remove again low molecule, the methyl ethylene organosilicon hydrolyzation thing that to obtain viscosity be 15mPas.
2) preparation of basic glue:
75kg octamethylcyclotetrasiloxane and 25kg octaphenylcyclotetrasiloxane and 25kg dimethyldiethoxysilane are joined in the polymerizer with devices such as stirring, thermometer, heating, vacuum, under the effect of 0.2kg Tetramethylammonium hydroxide alkali glue, under 125 ℃, reaction is 5 hours, then in same equipment, removes low molecule and makes balance silicone oil.Again balance silicone oil 100kg is moved in the glass lined reaction vessel with heating unit, add toluene 60kg and catalyzer hydrochloric acid (concentration is 36.5wt%) 0.5kg, at the refluxing toluene temperature, reaction is 4 hours, be cooled to room temperature water and be washed till neutrality, stratification, branch vibration layer, desolvation and low molecule, making viscosity is the oligomer that the 25mPas end group is hydroxyl.
In the polycondensation reactor with heating and vacuum unit, add above-mentioned oligomer 50kg, organosilicon hydrolyzation thing 50kg and dimethylbenzene 60kg, zinc octoate 0.03kg, carry out polycondensation at the refluxing xylene temperature, the low molecule removed in reaction reaches 0.8kg, decompression removes low molecule again, and obtaining viscosity is 10000mPas, the basic glue containing methyl, phenyl and vinyl that end group is hydroxyl.
3) preparation of the poly-ethylene methacrylic radical siloxane of platiniferous:
Add band stirring, temperature to take into account in the there-necked flask of reflux Platinic chloride 04kg and divinyl tetramethyl disiloxane 2kg, under the condition of 120 ℃, reaction is 2 hours, be washed till neutrality with deionized water, after dry 24 hours, be filled in poly-ethylene methacrylic radical siloxane 20kg, remove volatile matter, obtain 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 is added in the equipment with stirring and heating and vacuum system, and regulating mixing speed is 120 rev/mins, is warming up to 100 ℃, open vacuum pump, overbottom pressure 0.085Mpa, maintain 90 minutes, then be cooled to 60 ℃, add the poly-ethylene methacrylic radical siloxane 1.5kg of platiniferous and hydroxyl breast 0.1kg, maintain 60 minutes, cooling, through 120 order filtering nets, filter and package, obtain A component 99kg, its viscosity is at 13000mPas, and end group is hydroxyl;
By dibutyl tin laurate (0.3kg) packing, obtain the B component.
During use, after the B component is added in the A component to the row's of stirring evenly bubble, can pour into.Make the test piece performance as following table by this.
Table 4
Embodiment 4
1) preparation of organosilicon hydrolyzation thing:
Union carbide A-162, vinyltriethoxysilane, phenyl triethoxysilane are put into thermometer and stirring in 92: 3: 5 in molar ratio and dripped in the lass lining conversion unit of mouth, open and stir, add micro-hydrochloric acid, be warmed up to 80 ℃, drip deionized water, when after completion of the reaction, with sodium ethylate, neutralize neutrality, remove low molecule, obtaining viscosity is the organosilicon hydrolyzation thing containing methyl, vinyl and phenyl of 17mPas.
2) preparation of basic glue:
65kg octamethylcyclotetrasiloxane, 25kg octaphenylcyclotetrasiloxane and 10kg tetramethyl-tetrem thiazolinyl cyclotetrasiloxane and dimethyldiethoxysilane 25kg are joined in the polymerizer with devices such as stirring, thermometer, heating, vacuum, under the effect of 0.25kg catalyzer Tetramethylammonium hydroxide alkali glue, under 120 ℃, reaction is 5 hours, then in same equipment, removes low molecule and makes balance silicone oil.Again balance silicone oil 100kg is moved in the glass lined reaction vessel with heating unit, add toluene 60kg and 0.5kg hydrochloric acid (concentration is 36.5wt%), at the refluxing toluene temperature, reaction is 4 hours, be cooled to room temperature water and be washed till neutrality, stratification, branch vibration layer, desolvation and low molecule, making the viscosity that the end group containing phenyl, vinyl is hydroxyl is 30mPas organosilicon oligomer.
In the polycondensation reactor with heating and vacuum unit, add above-mentioned oligomer 50kg, organosilicon hydrolyzation thing 50kg and dimethylbenzene 60kg, octoate catalyst tin 0.03kg, carry out polycondensation at the refluxing xylene temperature, the low molecule removed in reaction reaches 0.75kg, decompression removes dimethylbenzene and low molecule again, and obtaining viscosity is 14000mPas, the basic glue containing phenyl and vinyl that end group is hydroxyl.
3) preparation of platiniferous methyl-silicone oil:
Add band stirring, temperature to take into account in the there-necked flask of reflux Platinic chloride 0.4kg and divinyl tetramethyl disiloxane 2kg, under the condition of 120 ℃, reaction is 2 hours, be washed till neutrality with deionized water, after dry 24 hours, be filled in polydimethylsiloxane 20kg, remove volatile matter, obtain faint yellow transparent platiniferous methylsiloxane.
4) preparation of the room temperature vulcanized silicone rubber of anti-ablation A component, B component:
Basic glue 99kg is added in the equipment with stirring and heating and vacuum system, and regulating mixing speed is 200 rev/mins, is warming up to 100 ℃, open vacuum pump, overbottom pressure 0.085Mpa, maintain 60～90 minutes, then be cooled to 60 ℃, add platiniferous methyl-silicone oil 1kg and deionized water 0.1kg, maintain 1 hour, cooling, through 120 order filtering nets, filter and package, obtain A component 99kg, end group is hydroxyl, and viscosity is 15800mPas.
By stannous octoate (0.3kg) packing, obtain the B component.
During use, after the B component is added in the A component to the row's of stirring evenly bubble, can pour into.Make the test piece performance as shown in the table.
Table 5
Embodiment 5
1) preparation of organosilicon hydrolyzation thing:
Union carbide A-162 and vinyltriethoxysilane (ratios of 8: 2 in molar ratio) are put into thermometer and stirring and dripped in the lass lining conversion unit of mouth, open and stir, add micro-hydrochloric acid, be warmed up to 80 ℃, drip deionized water, when after completion of the reaction, with sodium ethylate, be neutralized to neutrality, remove low molecule, obtaining viscosity is the organosilicon hydrolyzation thing containing methyl and vinyl of 14mPas.
2) preparation of basic glue:
In the polymerizer with devices such as stirring, thermometer, heating, vacuum, add octamethylcyclotetrasiloxane 100kg and dimethyldiethoxysilane 25kg, under the effect of catalyzer Tetramethylammonium hydroxide 0.2kg, under 110 ℃, reaction is 5 hours, then in same equipment, removes low molecule and makes balance silicone oil.Again balance silicone oil 100kg is moved in the glass lined reaction vessel with heating unit, add toluene 60kg and catalyzer hydrochloric acid (concentration is 36.5wt%) 0.5kg, at the refluxing toluene temperature, reaction is 4 hours, be cooled to room temperature water and be washed till neutrality, stratification, branch vibration layer, remove dimethylbenzene and low molecule, and making viscosity is the organosilicon oligomer that the 16mPas end group is hydroxyl.
In the polycondensation reactor with heating and vacuum unit, add above-mentioned oligomer 70KG, organosilicon hydrolyzation thing 30KG and dimethylbenzene 60kg, octoate catalyst zinc 0.03kg, carry out polycondensation at the refluxing xylene temperature, the low molecule removed in reaction reaches 0.75kg, decompression removes low molecule again, and obtaining viscosity is the basic glue that the 6300mPas end group is hydroxyl.
3) preparation of platiniferous phenyl silicone oil:
Add band stirring, temperature to take into account in the there-necked flask of reflux Platinic chloride 0.04kg and divinyl tetramethyl disiloxane 2kg, under the condition of 120 ℃, reaction is 2 hours, be washed till neutrality with deionized water, after dry 24 hours, be filled in poly-phenylbenzene dimethyl siloxane 2kg, remove volatile matter, obtain 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 is added in the equipment with stirring and heating and vacuum system, and regulating mixing speed is 180 rev/mins, is warming up to 100 ℃, open vacuum pump, overbottom pressure 0.085Mpa, maintain 3 hours, then be cooled to 60 ℃, add platiniferous phenyl silicone oil 3kg and hydroxy silicon oil 0.1kg, maintain 1 hour, cooling, through 120 order filtering nets, filter and package, obtain A component 99kg, viscosity is 8300mPas;
By stannous octoate 0.5kg packing, obtain the B component.
During use, after the B component is added in the A component to the row's of stirring evenly bubble, can pour into.This test piece performance is as following table.
Table 6
Claims (4)
1. the room temperature vulcanized silicone rubber of anti-the ablation, is characterized in that, by the component of following weight parts, made:
Described basic glue main chain one or more oligomers in being selected from poly-phenylbenzene dimethyl siloxane, poly-ethylene methacrylic radical siloxane and polydimethylsiloxane make with the organosilicon hydrolyzation thing copolymerization that contains one or more groups in methyl, vinyl and phenyl, gained multipolymer viscosity is between 6000mPa ﹒ s～16000mPa ﹒ s, and end group is hydroxyl;
Described flame retardant mixes with the polysiloxane of one or more groups containing in phenyl, methyl or vinyl to remove again and hangs down molecule and make by carry out complexing containing platinic compound and silicone oligomer;
Described vulcanization accelerator is selected from one or more in positive silicic acid tin, stannous octoate and dibutyl tin laurate;
Described auxiliary agent is selected from one or more in hydroxy silicon oil, polydimethylsiloxane, hydroxyl breast and deionized water.
2. the room temperature vulcanized silicone rubber of anti-ablation the as claimed in claim 1, is characterized in that, the viscosity of described oligomer is 12mPa ﹒ s～50mPa ﹒ s.
3. the room temperature vulcanized silicone rubber of anti-ablation the as claimed in claim 1, it is characterized in that, prepared by following method by the described organosilicon hydrolyzation thing containing one or more groups in methyl, vinyl and phenyl: the Ethoxysilane that will contain one or more groups in methyl, vinyl and phenyl, under Determining Micro Acid and certain temperature condition, carry out quantitative hydrolysis reaction, then neutralize with organic bases, then remove low molecule, filter and get final product; The viscosity of gained organosilicon hydrolyzation thing is 3.5mPa ﹒ s～35mPa ﹒ s.
4. the method for preparing the room temperature vulcanized silicone rubber of anti-ablation the claimed in claim 1, it is characterized in that, the basic glue of formula ratio is added in conversion unit, and in 50～100 ℃, stirring velocity is 120～300 rev/mins, under the condition of overbottom pressure 0.085Mpa, maintain 60～90 minutes, be cooled to 60 ℃, add flame retardant, the auxiliary agent of formula ratio, maintain 60～90 minutes, filter discharging as the A component; Vulcanization accelerator is as the B component, during use, the B component added in the A component after the row's of stirring evenly bubble, can pour into.
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| JP5004433B2 (en) * | 2005-04-27 | 2012-08-22 | 東レ・ダウコーニング株式会社 | Curable silicone composition and cured product thereof |
| CN101851334B (en) * | 2010-04-19 | 2011-11-30 | 上海爱世博有机硅材料有限公司 | Dimethyl diphenyl room-temperature vulcanized silicone rubber as well as production process and application thereof |
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| CN106190007B (en) * | 2016-07-22 | 2019-08-09 | 航天材料及工艺研究所 | A kind of room temperature curing electrically insulating silicone rubber of resistance to ablation adhesive and preparation method thereof |
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