CN102675667A - Preparation method of self-repairing POSS/microcapsule composite film - Google Patents
Preparation method of self-repairing POSS/microcapsule composite film Download PDFInfo
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Abstract
The invention relates to a preparation method of a composite film, particularly a preparation method of a self-repairing POSS/microcapsule composite film, which solves the technical problems generated by microcracking of microcapsules. The method comprises the following steps: 1. preparing a POSS gel; 2. preparing microcapsules; and 3. adding the microcapsules into polyamic acid to obtain a mixed solution, carrying out spin coating on a glass sheet, transferring the coated glass sheet into a baking oven, keeping the temperature at 80 DEG C for 30 minutes, keeping the temperature at 120 DEG C for 2 hours, and keeping the temperature at 130 DEG C for 30 minutes, thereby obtaining the self-repairing POSS/microcapsule composite film. The self-repairing POSS/microcapsule composite film can endow the inorganic nano material POSS with high rigidity, and can be quickly decomposed into SiO2 under high-temperature conditions, thereby gluing the microcracks and enhancing the mechanical properties of the film.
Description
Technical field
The present invention relates to a kind of preparation method of composite package.
Background technology
The metallic surface thermal protection technology all has crucial researching value and application space widely at aerospace, petrochemical complex, war industry and civil area.Usually adopt two big technological solar heat protection at present; One is to use the veneer of ceramic-like etc. to cover hull; Prevent the pyritous intrusion with this, also there are many deficiencies in this structure and material, like fragility, stream, high temperature absorption and maintenance difficult etc.; Thereby limited result of use, and indivedual solar heat protection watt fracture or obscission once took place; Two are to use the metal heat insulation material to be laid on the lagging material of hull surface, and it has lot of advantages: the requirement that intensity is high, plasticity is good, antifatigue, shaping surface are good, can guarantee pneumatic profile, can carry out damage tolerance design, the life-span is long, safety is big, flexible for installation, easy to maintenance etc.There are a lot of shortcomings simultaneously in this structure: the surface needs anti-oxidant radiation coating to protect; The oxidation on metal surface thing is to ionized air combined katalysis; Increase the thermal load of metallic surface; Thermal expansivity is high, is easy to produce thermal stresses and buckling deformation, and the difficult design of connection between the metal watt.The realization of heat release system function depends on top coat to a great extent, and top coat also is the important leverage of solar heat protection watt self structure integrity aspect the potential outside damage resisting.Though top coat can be high temperature resistant, receive the comprehensive action of various factors in the severe environment through repeatedly flying, it damages also unavoidable.No matter adopt which kind of technology, all be unable to do without lagging material.This type of material warp repeatedly is prone to tiny crack in the thermal cycling surface, and the existence of this crackle will cause that with expansion the intensity of material and toughness descend, and cause the member premature failure, even cause catastrophic failure.Along with developing rapidly of aerospace science and technology, more and more harsher to the requirement of lagging material, existing lagging material more and more can not satisfy the demand for development of multifunctional thermal-insulation technology.It is a research focus of lagging material applicating and exploitation that thermal protection is coated with, and one of its important development direction is the research and development of the compound lagging material of lower thermal conductivity.
Thermal protection coating can expand along with variation of temperature or shrink usually, thereby produces tiny crack.These tiny cracks can in use become greatly, and might expand as fatal crack, and the prevention of tiny crack also is the problem that must solve in the thermal protection coating development with repairing.If the intensity that can recover material is handled in the crackle self-healing, improve safety, increase the service life.
The thermally protective materials majority is pottery and ceramic matric composite; The unique texture of polyhedral oligomeric silsesquioxane POSS (polyhedral oligomeric silsesquioxance) is given this type of material and is had good mechanical and multiple properties such as thermal property, anti-atomic oxygen, anti-ablation and flame retardant resistance, and scientists is being explored its suitability at aerospace field at present.China's relevant report of relevant POSS in recent years also increases gradually, mainly concentrates on compound method and thermal property enhancing aspect.
Microcapsule are to utilize the material of film forming properties to coat the fine particle with " examining a shell " structure that has dispersed solid matter, drop or gas and form, and usually coating film are called cyst wall, and the material that film forming material inside is coated is called core.For avoiding the generation of coating internal tiny crack, the scientific research personnel has extensively carried out the research that contains the microencapsulation coating self-repair technology.
Summary of the invention
The objective of the invention is provides a kind of preparation method of self-repair type POSS/ microcapsule composite package in order to solve the technical problem that the microcapsule tiny crack produces.
The preparation method of self-repair type POSS/ microcapsule composite package is following:
One, the preparation of POSS colloidal sol: after 52g ethanol and 17.8g acetate mixed, join in the beaker that 55g silane coupling agent JH-60 is housed, stir, sealing is hydrolysis reaction 10 days under 30 ℃ the condition at bath temperature, obtains POSS colloidal sol;
Two, the 0.2g Z 150PH is joined in the 60g water dissolve, be cooled to room temperature, obtain polyvinyl alcohol solution;
Three, 10g POSS colloidal sol is joined in the 100g water, dissolve 0.2g～0.3g POSS colloidal sol at every turn and stir, get mixing solutions to dissolving the continued dissolving fully;
Four, the preparation of microcapsule: polyvinyl alcohol solution and 20g absolute ethyl alcohol are joined in the mixing solutions, stirred 2～3 minutes, leave standstill, promptly get microcapsule;
Five, 35 ℃ with 3,3 ', 4; 4 '-bibenzene tetracarboxylic dianhydride and 4,4 '-diaminodiphenyl oxide is dissolved in the DMAC N,N according to 1: 1 mol ratio; Process polyamic acid, then microcapsule are joined in the polyamic acid, obtain mixed solution; The massfraction of microcapsule is 5%～20% in the mixed solution; Be used in then and carry out spin-coating on the sheet glass, the sheet glass of filming is changed in the baking oven 2 hours, 130 ℃ constant temperature of 30 minutes, 120 ℃ constant temperature of 80 ℃ of constant temperature 30 minutes, promptly get self-repair type POSS/ microcapsule composite package.
Self-repair type POSS/ microcapsule of the present invention composite package-aspect organic/inorganic nano material POSS in addition has very high rigidity, and under hot conditions, can be decomposed into SiO rapidly
2, not only can gluing hallrcuts, and can improve the mechanical property of film.In addition, receive the interface chemistry principle, POSS hybrid material surface is coated with machine component Z 150PH, on the one hand solved the dispersiveness of POSS in polyimide, make it on the other hand under the intact condition of hull material, do not receive the influence of external environment.
Description of drawings
Fig. 1 is the fourier infrared graphic representation of used silane coupling agent JH-60 in the experiment one;
Fig. 2 is that experiment one gained self-repair type POSS/ microcapsule composite package amplifies 100 times shape appearance figure;
Fig. 3 tests the fourier infrared graphic representation of a step 5 gained polyamic acid;
Fig. 4 is a surface topography map after 400 ℃ of pyroprocessing of experiment one gained self-repair type POSS/ microcapsule composite package;
Fig. 5 is a surface topography map after 400 ℃ of pyroprocessing of experiment two gained self-repair type POSS/ microcapsule composite packages;
Fig. 6 is a surface topography map after 400 ℃ of pyroprocessing of experiment three gained self-repair type POSS/ microcapsule composite packages;
Fig. 7 is a surface topography map after 400 ℃ of pyroprocessing of experiment four gained self-repair type POSS/ microcapsule composite packages;
Fig. 8 is a surface topography map after 400 ℃ of pyroprocessing of experiment five gained self-repair type POSS/ microcapsule composite packages.
Embodiment
Technical scheme of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of this embodiment self-repair type POSS/ microcapsule composite package is following:
One, the preparation of POSS colloidal sol: after 52g ethanol and 17.8g acetate mixed, join in the beaker that 55g silane coupling agent JH-60 is housed, stir, sealing is hydrolysis reaction 10 days under 30 ℃ the condition at bath temperature, obtains POSS colloidal sol;
Two, the 0.2g Z 150PH is joined in the 60g water dissolve, be cooled to room temperature, obtain polyvinyl alcohol solution;
Three, 10g POSS colloidal sol is joined in the 100g water, dissolve 0.2g～0.3g POSS colloidal sol at every turn and stir, get mixing solutions to dissolving the continued dissolving fully;
Four, the preparation of microcapsule: polyvinyl alcohol solution and 20g absolute ethyl alcohol are joined in the mixing solutions, stirred 2～3 minutes, leave standstill, promptly get microcapsule;
Five, 35 ℃ with 3,3 ', 4; 4 '-bibenzene tetracarboxylic dianhydride and 4,4 '-diaminodiphenyl oxide is dissolved in the DMAC N,N according to 1: 1 mol ratio; Process polyamic acid, then microcapsule are joined in the polyamic acid, obtain mixed solution; The massfraction of microcapsule is 5%～20% in the mixed solution; Be used in then and carry out spin-coating on the sheet glass, the sheet glass of filming is changed in the baking oven 2 hours, 130 ℃ constant temperature of 30 minutes, 120 ℃ constant temperature of 80 ℃ of constant temperature 30 minutes, promptly get self-repair type POSS/ microcapsule composite package.
Embodiment two: this embodiment and embodiment one are different is that the massfraction of microcapsule in the mixed solution described in the step 5 is 10%.Other is identical with embodiment one.
Embodiment three: this embodiment and embodiment one are different is that the massfraction of microcapsule in the mixed solution described in the step 5 is 15%.Other is identical with embodiment one.
Adopt following experimental verification effect of the present invention:
Experiment one:
The preparation method of self-repair type POSS/ microcapsule composite package is following:
One, the preparation of POSS colloidal sol: after 52g ethanol and 17.8g acetate mixed, join in the beaker that 55g silane coupling agent JH-60 is housed, stir, sealing is hydrolysis reaction 10 days under 30 ℃ the condition at bath temperature, obtains POSS colloidal sol;
Two, the 0.2g Z 150PH is joined in the 60g water dissolve, be cooled to room temperature, obtain polyvinyl alcohol solution;
Three, 10g POSS colloidal sol is joined in the 100g water, dissolve 0.2g～0.3g POSS colloidal sol at every turn and stir, get mixing solutions to dissolving the continued dissolving fully;
Four, the preparation of microcapsule: polyvinyl alcohol solution and 20g absolute ethyl alcohol are joined in the mixing solutions, stirred 2～3 minutes, leave standstill, promptly get microcapsule;
Five, 35 ℃ with 3,3 ', 4; 4 '-bibenzene tetracarboxylic dianhydride and 4,4 '-diaminodiphenyl oxide is dissolved in the DMAC N,N according to 1: 1 mol ratio; Process polyamic acid, then microcapsule are joined in the polyamic acid, obtain mixed solution; The massfraction of microcapsule is 5% in the mixed solution; Be used in then and carry out spin-coating on the sheet glass, the sheet glass of filming is changed in the baking oven 2 hours, 130 ℃ constant temperature of 30 minutes, 120 ℃ constant temperature of 80 ℃ of constant temperature 30 minutes, promptly get self-repair type POSS/ microcapsule composite package.
Experiment two:
The preparation method of self-repair type POSS/ microcapsule composite package is following:
One, the preparation of POSS colloidal sol: after 52g ethanol and 17.8g acetate mixed, join in the beaker that 55g silane coupling agent JH-60 is housed, stir, sealing is hydrolysis reaction 10 days under 30 ℃ the condition at bath temperature, obtains POSS colloidal sol;
Two, the 0.2g Z 150PH is joined in the 60g water dissolve, be cooled to room temperature, obtain polyvinyl alcohol solution;
Three, 10g POSS colloidal sol is joined in the 100g water, dissolve 0.2g～0.3g POSS colloidal sol at every turn and stir, get mixing solutions to dissolving the continued dissolving fully;
Four, the preparation of microcapsule: polyvinyl alcohol solution and 20g absolute ethyl alcohol are joined in the mixing solutions, stirred 2～3 minutes, leave standstill, promptly get microcapsule;
Five, 35 ℃ with 3,3 ', 4; 4 '-bibenzene tetracarboxylic dianhydride and 4,4 '-diaminodiphenyl oxide is dissolved in the DMAC N,N according to 1: 1 mol ratio; Process polyamic acid, then microcapsule are joined in the polyamic acid, obtain mixed solution; The massfraction of microcapsule is 10% in the mixed solution; Be used in then and carry out spin-coating on the sheet glass, the sheet glass of filming is changed in the baking oven 2 hours, 130 ℃ constant temperature of 30 minutes, 120 ℃ constant temperature of 80 ℃ of constant temperature 30 minutes, promptly get self-repair type POSS/ microcapsule composite package.
Experiment three:
The preparation method of self-repair type POSS/ microcapsule composite package is following:
One, the preparation of POSS colloidal sol: after 52g ethanol and 17.8g acetate mixed, join in the beaker that 55g silane coupling agent JH-60 is housed, stir, sealing is hydrolysis reaction 10 days under 30 ℃ the condition at bath temperature, obtains POSS colloidal sol;
Two, the 0.2g Z 150PH is joined in the 60g water dissolve, be cooled to room temperature, obtain polyvinyl alcohol solution;
Three, 10g POSS colloidal sol is joined in the 100g water, dissolve 0.2g～0.3g POSS colloidal sol at every turn and stir, get mixing solutions to dissolving the continued dissolving fully;
Four, the preparation of microcapsule: polyvinyl alcohol solution and 20g absolute ethyl alcohol are joined in the mixing solutions, stirred 2～3 minutes, leave standstill, promptly get microcapsule;
Five, 35 ℃ with 3,3 ', 4; 4 '-bibenzene tetracarboxylic dianhydride and 4,4 '-diaminodiphenyl oxide is dissolved in the DMAC N,N according to 1: 1 mol ratio; Process polyamic acid, then microcapsule are joined in the polyamic acid, obtain mixed solution; The massfraction of microcapsule is 15% in the mixed solution; Be used in then and carry out spin-coating on the sheet glass, the sheet glass of filming is changed in the baking oven 2 hours, 130 ℃ constant temperature of 30 minutes, 120 ℃ constant temperature of 80 ℃ of constant temperature 30 minutes, promptly get self-repair type POSS/ microcapsule composite package.
Experiment four:
The preparation method of self-repair type POSS/ microcapsule composite package is following:
One, the preparation of POSS colloidal sol: after 52g ethanol and 17.8g acetate mixed, join in the beaker that 55g silane coupling agent JH-60 is housed, stir, sealing is hydrolysis reaction 10 days under 30 ℃ the condition at bath temperature, obtains POSS colloidal sol;
Two, the 0.2g Z 150PH is joined in the 60g water dissolve, be cooled to room temperature, obtain polyvinyl alcohol solution;
Three, 10g POSS colloidal sol is joined in the 100g water, dissolve 0.2g～0.3g POSS colloidal sol at every turn and stir, get mixing solutions to dissolving the continued dissolving fully;
Four, the preparation of microcapsule: polyvinyl alcohol solution and 20g absolute ethyl alcohol are joined in the mixing solutions, stirred 2～3 minutes, leave standstill, promptly get microcapsule;
Five, 35 ℃ with 3,3 ', 4; 4 '-bibenzene tetracarboxylic dianhydride and 4,4 '-diaminodiphenyl oxide is dissolved in the DMAC N,N according to 1: 1 mol ratio; Process polyamic acid, then microcapsule are joined in the polyamic acid, obtain mixed solution; The massfraction of microcapsule is 20% in the mixed solution; Be used in then and carry out spin-coating on the sheet glass, the sheet glass of filming is changed in the baking oven 2 hours, 130 ℃ constant temperature of 30 minutes, 120 ℃ constant temperature of 80 ℃ of constant temperature 30 minutes, promptly get self-repair type POSS/ microcapsule composite package.
Experiment five:
The preparation method of self-repair type POSS/ microcapsule composite package is following:
One, the preparation of POSS colloidal sol: after 52g ethanol and 17.8g acetate mixed, join in the beaker that 55g silane coupling agent JH-60 is housed, stir, sealing is hydrolysis reaction 10 days under 30 ℃ the condition at bath temperature, obtains POSS colloidal sol;
Two, the 0.2g Z 150PH is joined in the 60g water dissolve, be cooled to room temperature, obtain polyvinyl alcohol solution;
Three, 10g POSS colloidal sol is joined in the 100g water, dissolve 0.2g～0.3g POSS colloidal sol at every turn and stir, get mixing solutions to dissolving the continued dissolving fully;
Four, the preparation of microcapsule: polyvinyl alcohol solution and 20g absolute ethyl alcohol are joined in the mixing solutions, stirred 2～3 minutes, leave standstill, promptly get microcapsule;
Five, 35 ℃ with 3,3 ', 4; 4 '-bibenzene tetracarboxylic dianhydride and 4,4 '-diaminodiphenyl oxide is dissolved in the DMAC N,N according to 1: 1 mol ratio; Process polyamic acid, then microcapsule are joined in the polyamic acid, obtain mixed solution; The massfraction of microcapsule is 0% in the mixed solution; Be used in then and carry out spin-coating on the sheet glass, the sheet glass of filming is changed in the baking oven 2 hours, 130 ℃ constant temperature of 30 minutes, 120 ℃ constant temperature of 80 ℃ of constant temperature 30 minutes, promptly get self-repair type POSS/ microcapsule composite package.
Claims (3)
1. the preparation method of self-repair type POSS/ microcapsule composite package is characterized in that the preparation method of self-repair type POSS/ microcapsule composite package is following:
One, the preparation of POSS colloidal sol: after 52g ethanol and 17.8g acetate mixed, join in the beaker that 55g silane coupling agent JH-60 is housed, stir, sealing is hydrolysis reaction 10 days under 30 ℃ the condition at bath temperature, obtains POSS colloidal sol;
Two, the 0.2g Z 150PH is joined in the 60g water dissolve, be cooled to room temperature, obtain polyvinyl alcohol solution;
Three, 10g POSS colloidal sol is joined in the 100g water, dissolve 0.2g～0.3g POSS colloidal sol at every turn and stir, get mixing solutions to dissolving the continued dissolving fully;
Four, the preparation of microcapsule: polyvinyl alcohol solution and 20g absolute ethyl alcohol are joined in the mixing solutions, stirred 2～3 minutes, leave standstill, promptly get microcapsule;
Five, 35 ℃ with 3,3 ', 4; 4 '-bibenzene tetracarboxylic dianhydride and 4,4 '-diaminodiphenyl oxide is dissolved in the DMAC N,N according to 1: 1 mol ratio; Process polyamic acid, then microcapsule are joined in the polyamic acid, obtain mixed solution; The massfraction of microcapsule is 5%～20% in the mixed solution; Be used in then and carry out spin-coating on the sheet glass, the sheet glass of filming is changed in the baking oven 2 hours, 130 ℃ constant temperature of 30 minutes, 120 ℃ constant temperature of 80 ℃ of constant temperature 30 minutes, promptly get self-repair type POSS/ microcapsule composite package.
2. according to the preparation method of the said self-repair type POSS/ of claim 1 microcapsule composite package, the massfraction that it is characterized in that microcapsule in the mixed solution described in the step 5 is 10%.
3. according to the preparation method of the said self-repair type POSS/ of claim 1 microcapsule composite package, the massfraction that it is characterized in that microcapsule in the mixed solution described in the step 5 is 15%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103275587A (en) * | 2013-06-18 | 2013-09-04 | 哈尔滨工业大学 | Preparation method for antistatic synthetic glass film |
| CN104892843A (en) * | 2015-06-16 | 2015-09-09 | 厦门大学 | POSS (polyhedral oligomeric silsesquioxane)-group-containing comb polymer with self-repairing function and preparation method of comb polymer |
| CN106345320A (en) * | 2016-09-14 | 2017-01-25 | 天津大学 | Hollow fiber ceramic membrane preparation method |
| CN109675446A (en) * | 2017-10-18 | 2019-04-26 | 中国石油化工股份有限公司 | A kind of super hydrophilic modified polyvinilidene fluoride film and the preparation method and application thereof |
| CN111001363A (en) * | 2019-11-15 | 2020-04-14 | 温州科技职业学院 | Preparation method of high-mechanical-strength nano microcapsule with insect-trapping function |
| CN113980465A (en) * | 2021-12-13 | 2022-01-28 | Tcl华星光电技术有限公司 | Polyimide film, flexible display screen and preparation method thereof |
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| CN101431157A (en) * | 2007-11-07 | 2009-05-13 | 国立大学法人静冈大学 | Electrolyte membrane for fuel cell |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103275587A (en) * | 2013-06-18 | 2013-09-04 | 哈尔滨工业大学 | Preparation method for antistatic synthetic glass film |
| CN104892843A (en) * | 2015-06-16 | 2015-09-09 | 厦门大学 | POSS (polyhedral oligomeric silsesquioxane)-group-containing comb polymer with self-repairing function and preparation method of comb polymer |
| CN106345320A (en) * | 2016-09-14 | 2017-01-25 | 天津大学 | Hollow fiber ceramic membrane preparation method |
| CN109675446A (en) * | 2017-10-18 | 2019-04-26 | 中国石油化工股份有限公司 | A kind of super hydrophilic modified polyvinilidene fluoride film and the preparation method and application thereof |
| CN111001363A (en) * | 2019-11-15 | 2020-04-14 | 温州科技职业学院 | Preparation method of high-mechanical-strength nano microcapsule with insect-trapping function |
| CN111001363B (en) * | 2019-11-15 | 2021-11-02 | 温州科技职业学院 | Preparation method of high-mechanical-strength nano microcapsule with insect-trapping function |
| CN113980465A (en) * | 2021-12-13 | 2022-01-28 | Tcl华星光电技术有限公司 | Polyimide film, flexible display screen and preparation method thereof |
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