CN102863723A - Organosilicone resin composition serving as propulsive agent to wrap transition layer and steeping wrapping layer and preparation method thereof - Google Patents
Organosilicone resin composition serving as propulsive agent to wrap transition layer and steeping wrapping layer and preparation method thereof Download PDFInfo
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- CN102863723A CN102863723A CN2012103606353A CN201210360635A CN102863723A CN 102863723 A CN102863723 A CN 102863723A CN 2012103606353 A CN2012103606353 A CN 2012103606353A CN 201210360635 A CN201210360635 A CN 201210360635A CN 102863723 A CN102863723 A CN 102863723A
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Abstract
The invention discloses an organosilicone resin composition serving as a propulsive agent to wrap a transition layer and a steeping wrapping layer and a preparation method of the organosilicone resin composition. The organosilicone resin composition is prepared by mixing a butyl methacrylate-organosilicone monomer copolymer toluene solution in the content of 50%, aluminum hydroxide and a metal organic acid salt catalyst according to mass percentage of 70-90:9.5-25:0.5-5. Simultaneously, the invention further provides a preparation method of the butyl methacrylate-organosilicone monomer copolymer toluene solution. The organosilicone resin composition can serve as the propulsive agent to wrap the transition layer and the steeping wrapping layer, has good bonding performance, burning corrosion performance, compatibility and solvent resistance, is low in fuming quantity, does not contain elements such as halogen and phosphorus and the like and is low in degree of harm and pollution of human bodies and environment due to the fact that products resolved by burning is free of toxin.
Description
Technical field
The present invention relates to propelling agent coating material technical field, is a kind of organosilicon resin composition and preparation method who coats transition layer and dipping coating layer as propelling agent specifically.
Background technology
Coating layer is the weight integral part more of solid rocket propellant powder charge.Its basic role is the burning area of control propellant charge, plays again the heat-blocking action to motor body simultaneously; Its performance is determining working order and the work-ing life of rocket engine.Along with improving constantly of rocketry, multiple macromolecular material is applied to coating.
At present, research mainly contains urethane, unsaturated polyester, silicon rubber, terpolymer EP rubber etc. with the coating material of using.German Patent report polycaprolactone and PTMG are the urethane of raw material preparation, this class urethane has preferably anti-hydrolytic performance, in system, add gasifiable filler (such as oxamide) and ester plasticizer, available can excellent urethane coating layer (Ger 3 517 892,1985).Unsaturated polyester material has intensity height, transparent, can under normal temperature environment, solidify and solidification process in no coupling product, bonding reliable with double-basis, composite modified double base propellant, the advantage such as cladding process is simple and cheap is widely applied in the coating of double-base propellent.But, Cured up resin exist fragility large, differ larger shortcoming with the propelling agent coefficient of linear expansion, have a strong impact on and propelling agent between mechanical property coupling, especially its low temperature unit elongation is lower, and the range of application of powder charge is caused to a certain degree restriction.The domestic and international research that Silicone Rubber Inhibitor is carried out comprises the aspects such as modification, the prescription to the basic glue of silicon rubber chosen, adhesive property.But the silicon rubber adhesive property is reliable and stable not, and its application is subject to certain limitation.Terpolymer EP rubber has obtained using more and more widely with its low density, anti-ablation, the advantage such as ageing-resistant, can satisfy the technical requirements of engine combustion chamber interior walls thermal insulation layer, but adhesiveproperties poor (aerospace material technique, 2005,1:39-41).
Coating layer can be one deck, also can be multilayer, and every layer effect is different.For example, the powder charge that has is having tack coat between thermal insulation layer and the coating layer or between coating layer and the propelling agent; Between coating layer and propelling agent for preventing that plasticizer migration from setting up the blocking layer; On coating layer, add again one deck coating layer to eliminate internal stress or physical abuse etc.The material with difference in functionality that applies between propelling agent and the coating layer is referred to as transition layer.Daume proposes a kind of by 20 parts of tritanes 4,4 ', 4 " triisocyanate, 80 parts of methylene dichloride, 10～100 parts of transition layers that N-BUTYL ACETATE forms, the urea groups of low molecule triisocyanate and airborne water reaction generation high concentration; form blocking layer (US 4 034 676,1977).
Common coating technology has dipping coating, casting coating, paster coating etc.It is to dry after powder column is placed coating solution dipping that dipping coats, to form the technique of certain thickness coating layer.
Along with the development of double-base propellent, composite modified double base propellant and compositepropellent, coating layer to be had higher requirement, the macromolecular material of namely selecting must satisfy the performance of coating layer, thereby makes the performance of solid propellant constantly be improved and improve.The present invention has good adhesive property, ablation resistance, consistency, solvent resistance as the organosilicon resin composition that propelling agent coats transition layer and dipping coating layer, low-smoke, the element such as Halogen, phosphorus not, combustion decomposition product nontoxicity is low to harm and the pollution level of human body and environment.
Summary of the invention
The purpose of this invention is to provide a kind of organosilicon resin composition that coats transition layer and dipping coating layer as propelling agent, be intended to overcome the deficiencies in the prior art, it has good adhesive property, ablation resistance, consistency, solvent resistance, low-smoke, the element such as Halogen, phosphorus not, combustion decomposition product nontoxicity is low to harm and the pollution level of human body and environment.
Another object of the present invention provides a kind of preparation method of above-mentioned organosilicon resin composition.
Realize that technical solution of the present invention is: a kind of organosilicon resin composition that coats transition layer and dipping coating layer as propelling agent, formed by butyl methacrylate-organosilane monomer multipolymer toluene solution, aluminium hydroxide and metal organic acid salt catalyst mix, the mass percent of butyl methacrylate-organosilane monomer multipolymer toluene solution, aluminium hydroxide and metal organic acid salt catalyst is (70 ~ 90): (9.5 ~ 25): (0.5 ~ 5); Wherein butyl methacrylate-the mass concentration of organosilane monomer multipolymer in toluene solution is 50%, the consisting of of butyl methacrylate-organosilane monomer multipolymer: 70wt% butyl methacrylate, 20wt%KH570 and 10wt%KH571.
Described metal organic acid salt catalyst is selected from a kind of in dibutyl tin dilaurate, dibutyl tin acetate or the stannous iso caprylate.
A kind of method for preparing the above-mentioned organosilicon resin composition that is used as propelling agent coating transition layer and dipping coating layer, be by mass percentage 70 ~ 90:9.5 ~ 25:0.5 ~ 5 with toluene solution, aluminium hydroxide and metal organic acid salt catalyst mix, the stirring of butyl methacrylate-organosilane monomer multipolymer, prepare described composition.
The organosilicon resin composition that coats transition layer and dipping coating layer as propelling agent of the present invention compared with prior art has obvious progress.(1) adopt butyl methacrylate-organosilane monomer multipolymer as body material, the elemental silicon of anti-the ablation is introduced polymer architecture, changed the polymer cracking mode, form essential ablation resistant material, anti-ablation is effective.(2) add filling aluminium hydrate, undertaken crosslinkedly by silicon-containing monomer and surface of aluminum hydroxide hydroxyl reaction, reach anti-solvent, effect that consistency is good.(3) KH570 and KH571 are introduced in the macromolecular chain, form macromolecular coupling agent, in the macromole oxyalkylene segment can with propelling agent in soluble cotton etc. have an effect, the butyl methacrylate chain link can form Intermolecular Forces with the low material of polarity, thereby reaches good cohesive strength.(4) composition is the fatty compounds system, and the carbon-to-oxygen ratio value is close to 1, and the amount of being fuming is few.(5) this material Halogen, without phosphorus, the combustion decomposition product is little on the human and environment impact.
Embodiment
Of the present inventionly coating the organosilicon resin composition of transition layer and dipping coating layer as propelling agent, is that 50% the butyl methacrylate-toluene solution of organosilane monomer multipolymer, aluminium hydroxide, metal organic acid salt catalyst mix form by content.
Organosilicon resin composition preparation method as propelling agent coating transition layer and dipping coating layer of the present invention is as follows, be 70 ~ 90:9.5 ~ 25:0.5 ~ 5 by mass percentage with the butyl methacrylate of 50wt%-toluene solution, aluminium hydroxide and the metal organic acid salt catalyst mix of organosilane monomer multipolymer, stirring, be prepared into the organosilicon resin composition that coats transition layer and dipping coating layer as propelling agent.The aluminium hydroxide particle diameter is between 1～20 μ m.Describe the preparation process that coats the organosilicon resin composition of transition layer and dipping coating layer as propelling agent in detail below in conjunction with embodiment.
The preparation method of the toluene solution of butyl methacrylate of the present invention-organosilane monomer multipolymer, concrete steps are as follows:
Take by weighing 42g butyl methacrylate, 12gKH570,6gKH571,100g toluene and 1.2g Diisopropyl azodicarboxylate and drop in the there-necked flask, heating is also stirred, in 80 ~ 90
oBecome sticky to solution about backflow 1h under the C, take by weighing again 28g butyl methacrylate, 8 gKH570,4gKH571 and 0.8g Diisopropyl azodicarboxylate, be added drop-wise in the there-necked flask after the mixing, the control rate of addition, about 40min drips off, the 1.5h that refluxes again after dripping off, the toluene solution of multipolymer is finished to get in polymerization, and viscosity is between 380 ~ 3000cps under the room temperature.
Embodiment 1:
Get the toluene solution 80g of the butyl methacrylate that contains 50wt%-organosilane monomer multipolymer, aluminium hydroxide 17g, catalyzer dibutyl tin dilaurate 3g mixes, stirs 15min, and preparation coats the organosilicon resin composition of transition layer and dipping coating layer as propelling agent.
Propellant charge is surperficial with 1
#Sand papering, the acetone degreasing.Dipping the organosilicon resin composition that coats transition layer and dipping coating layer as propelling agent with brush brushes toward propellant charge from a direction, after brush is gone over, 5min dries in the air, brush again second time, 5min again dries in the air, brush again the 3rd time, or the organosilicon resin composition dipping that powder column is immersed as propelling agent coating transition layer and dipping coating layer coats.7 angel's transition layers or coating layer solidify with drying in the air in the powder column holding chamber.Performance sees Table 1.
Embodiment 2:
Get the toluene solution 85g of the butyl methacrylate that contains 50wt%-organosilane monomer multipolymer, aluminium hydroxide 13g, catalyzer dibutyl tin acetate 2g mixes, stirs 15min, and preparation coats the organosilicon resin composition of transition layer and dipping coating layer as propelling agent.
Propellant charge is surperficial with 1
#Sand papering, the acetone degreasing.Dipping the organosilicon resin composition that coats transition layer and dipping coating layer as propelling agent with brush brushes toward powder column from a direction, after brush is gone over, 5min dries in the air, brush again second time, 5min again dries in the air, brush again the 3rd time, or the organosilicon resin composition dipping that propelling agent is immersed as propelling agent coating transition layer and dipping coating layer coats.7 angel's transition layers or coating layer solidify with drying in the air in the powder column holding chamber.Performance sees Table 1.
Embodiment 3:
Get the toluene solution 75g of the butyl methacrylate that contains 50wt%-organosilane monomer multipolymer, aluminium hydroxide 23g, catalyzer dibutyl tin dilaurate 2g mixes, stirs 15min, and preparation coats the organosilicon resin composition of transition layer and dipping coating layer as propelling agent.
Propellant charge is surperficial with 1
#Sand papering, the acetone degreasing.Dipping the organosilicon resin composition that coats transition layer and dipping coating layer as propelling agent with brush brushes toward powder column from a direction, after brush is gone over, 5min dries in the air, brush again second time, 5min again dries in the air, brush again the 3rd time, or the organosilicon resin composition dipping that propelling agent is immersed as propelling agent coating transition layer and dipping coating layer coats.7 angel's transition layers or coating layer solidify with drying in the air in the powder column holding chamber.Performance sees Table 1.
Embodiment 4:
Get the toluene solution 90g of the butyl methacrylate that contains 50wt%-organosilane monomer multipolymer, aluminium hydroxide 9.5g, catalyzer stannous iso caprylate 0.5g mixes, stirs 15min, and preparation coats the organosilicon resin composition of transition layer and dipping coating layer as propelling agent.
Propellant charge is surperficial with 1
#Sand papering, the acetone degreasing.Dipping the organosilicon resin composition that coats transition layer and dipping coating layer as propelling agent with brush brushes toward powder column from a direction, after brush is gone over, 5min dries in the air, brush again second time, 5min again dries in the air, brush again the 3rd time, or the organosilicon resin composition dipping that propelling agent is immersed as propelling agent coating transition layer and dipping coating layer coats.7 angel's transition layers or coating layer solidify with drying in the air in the powder column holding chamber.Performance sees Table 1.
Embodiment 5:
Get the toluene solution 70g of the butyl methacrylate that contains 50wt%-organosilane monomer multipolymer, aluminium hydroxide 25g, catalyzer stannous iso caprylate 5g mixes, stirs 15min, and preparation coats the organosilicon resin composition of transition layer and dipping coating layer as propelling agent.
Propellant charge is surperficial with 1
#Sand papering, the acetone degreasing.Dipping the organosilicon resin composition that coats transition layer and dipping coating layer as propelling agent with brush brushes toward powder column from a direction, after brush is gone over, 5min dries in the air, brush again second time, 5min again dries in the air, brush again the 3rd time, or the organosilicon resin composition dipping that propelling agent is immersed as propelling agent coating transition layer and dipping coating layer coats.7 angel's transition layers or coating layer solidify with drying in the air in the powder column holding chamber.Performance sees Table 1.
Table 1 organosilicon resin composition performance
According to GB GB/T15814.3-1995, adopt differential thermal analysis (DTA) to measure the consistency of organosilicon resin composition and propelling agent.Whether solvent resistance: be brushed with outside powder column or after the organosilicon resin composition that floods solidifies, put it in the butyl methacrylate, observe in the 24h transition layer or coating layer and change, "-" expression does not change.Shearing resistance is measured according to GB/T 13936-92.Linear ablation rate is pressed GJB323A-96 and is measured.
Claims (6)
1. the organosilicon resin composition as propelling agent coating transition layer and dipping coating layer is characterized in that described composition is formed by butyl methacrylate-organosilane monomer multipolymer toluene solution, aluminium hydroxide and metal organic acid salt catalyst mix; The mass percent of butyl methacrylate-organosilane monomer multipolymer toluene solution, aluminium hydroxide and metal organic acid salt catalyst is (70 ~ 90): (9.5 ~ 25): (0.5 ~ 5); Wherein said butyl methacrylate-the mass concentration of organosilane monomer multipolymer in toluene solution is 50%, the consisting of of described butyl methacrylate-organosilane monomer multipolymer: 70wt% butyl methacrylate, 20wt%KH570 and 10wt%KH571.
2. the organosilicon resin composition as propelling agent coating transition layer and dipping coating layer according to claim 1 is characterized in that described metal organic acid salt catalyst is selected from a kind of of dibutyl tin dilaurate, dibutyl tin acetate or stannous iso caprylate.
3. the organosilicon resin composition as propelling agent coating transition layer and dipping coating layer according to claim 1 is characterized in that the particle diameter of described aluminium hydroxide is between 1～20 μ m.
4. one kind is used as the preparation method that propelling agent coats the organosilicon resin composition of transition layer and dipping coating layer, it is characterized in that described method is is that 70 ~ 90:9.5 ~ 25:0.5 ~ 5 are with butyl methacrylate-organosilane monomer multipolymer toluene solution by mass percentage, aluminium hydroxide and metal organic acid salt catalyst mix, stir, prepare described composition, wherein said butyl methacrylate-the mass concentration of organosilane monomer multipolymer in toluene solution is 50%, the consisting of of described butyl methacrylate-organosilane monomer multipolymer: the 70wt% butyl methacrylate, 20wt%KH570 and 10wt%KH571.
5. according to claim 4ly coat the preparation method of the organosilicon resin composition of transition layer and dipping coating layer as propelling agent, it is characterized in that described metal organic acid salt catalyst is selected from a kind of in dibutyl tin dilaurate, dibutyl tin acetate or the stannous iso caprylate.
6. the preparation method as propelling agent coating transition layer and the organosilicon resin composition of dipping coating layer according to claim 4 is characterized in that the particle diameter of described aluminium hydroxide is between 1～20 μ m.
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| CN2012103606353A CN102863723A (en) | 2012-09-25 | 2012-09-25 | Organosilicone resin composition serving as propulsive agent to wrap transition layer and steeping wrapping layer and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106593695A (en) * | 2016-12-15 | 2017-04-26 | 晋西工业集团有限责任公司 | Integral type nonmetal rocket engine empty body machining process |
| CN106812628A (en) * | 2016-12-15 | 2017-06-09 | 晋西工业集团有限责任公司 | A kind of nonmetallic engine sky body of monoblock type and its heat insulation layer synchronous forming technique |
| CN107434889A (en) * | 2017-09-20 | 2017-12-05 | 西安近代化学研究所 | A kind of low cigarette EPDM clad |
| CN110701964A (en) * | 2019-09-25 | 2020-01-17 | 宜宾北方川安化工有限公司 | Coating method of non-linear cylinder explosive column |
| CN112391002A (en) * | 2019-08-16 | 2021-02-23 | 南京理工大学 | Heat-shrinkable coating layer for solid propellant and preparation method thereof |
| CN115466437A (en) * | 2022-09-02 | 2022-12-13 | 山西北方兴安化学工业有限公司 | High-temperature-resistant flame-retardant coating material and preparation method thereof |
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2012
- 2012-09-25 CN CN2012103606353A patent/CN102863723A/en active Pending
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106593695A (en) * | 2016-12-15 | 2017-04-26 | 晋西工业集团有限责任公司 | Integral type nonmetal rocket engine empty body machining process |
| CN106812628A (en) * | 2016-12-15 | 2017-06-09 | 晋西工业集团有限责任公司 | A kind of nonmetallic engine sky body of monoblock type and its heat insulation layer synchronous forming technique |
| CN106812628B (en) * | 2016-12-15 | 2018-06-12 | 晋西工业集团有限责任公司 | A kind of nonmetallic engine hollow body of monoblock type and its heat insulation layer synchronous forming technique |
| CN107434889A (en) * | 2017-09-20 | 2017-12-05 | 西安近代化学研究所 | A kind of low cigarette EPDM clad |
| CN112391002A (en) * | 2019-08-16 | 2021-02-23 | 南京理工大学 | Heat-shrinkable coating layer for solid propellant and preparation method thereof |
| CN112391002B (en) * | 2019-08-16 | 2022-05-27 | 南京理工大学 | Heat-shrinkable coating layer for solid propellant and preparation method thereof |
| CN110701964A (en) * | 2019-09-25 | 2020-01-17 | 宜宾北方川安化工有限公司 | Coating method of non-linear cylinder explosive column |
| CN115466437A (en) * | 2022-09-02 | 2022-12-13 | 山西北方兴安化学工业有限公司 | High-temperature-resistant flame-retardant coating material and preparation method thereof |
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Application publication date: 20130109 |