CN110452409A - A kind of transparent meso silicon elastomeric precursor and preparation method thereof - Google Patents
A kind of transparent meso silicon elastomeric precursor and preparation method thereof Download PDFInfo
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- CN110452409A CN110452409A CN201910763078.1A CN201910763078A CN110452409A CN 110452409 A CN110452409 A CN 110452409A CN 201910763078 A CN201910763078 A CN 201910763078A CN 110452409 A CN110452409 A CN 110452409A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
- C08J2201/0502—Elimination by evaporation or heat degradation of a liquid phase the liquid phase being organic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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Abstract
The invention discloses a kind of transparent meso silicon elastomeric precursors and preparation method thereof.The transparent meso silicon elastomeric precursor is with hydroxyl-terminated injecting two methyl siloxane (PDMS-OH) and organosiloxane [Si (OR)4] it is raw material, Silica hydrogel is prepared by sol-gel chemistry method first；Through processes such as aging, washings；A kind of transparency for most preparing afterwards through special drying process is high, the porous organic elastomeric precursor with meso-hole structure.The transparency of the transparent meso silicon elastomeric precursor is from 50%-80%, density 300g/m3‑700g/m3, elasticity modulus is from 1MPa-20MPa etc., in addition, the transparent meso silicon elastomeric precursor has excellent bio-compatibility, continuous porous structure, specific surface area is up to 100m2/ g is with a wide range of applications in industries such as special type protection, industry, transport, food and drink, medicine.
Description
Technical field
The present invention relates to a kind of transparent, continuous poriferous organosilicone elastic precursors and preparation method thereof, belong to new type rubber
Materials synthesis field.
Background technique
Rubber is a kind of high resiliency high molecular material with reversible deformation, and usually high resilience at room temperature is and fibre
Dimension, plastics one of three big polymer materials arranged side by side, in communications and transportation, industry, agriculture, forestry, water conservancy, military affairs, civil construction, electrical logical
The wide range of areas such as news, health care, commodity storage and daily necessity play the effect that can not be substituted.By different classification sides
Method, rubber can be divided into variety classes and play unique effect in different application field.Such as by raw material sources, rubber can
It is divided into natural rubber and synthetic rubber two major classes；By mode of appearance, rubber can be divided into solid rubber, emulsus rubber, liquid rubber
With powdered rubber etc.；By physical aspect, rubber can be divided into ebonite and flexible glue, raw rubber and rubber compound etc.；By performance and purposes, rubber
General and specific rubber can be divided into.Wherein, silicon rubber refers to that main chain is alternately made of silicon and oxygen atom, is usually connected on silicon atom
The rubber of two organic groups.Silicon rubber resistance to low temperature is good, and use scope can instantaneously be resistant to 300 from -73 DEG C to 200 DEG C
DEG C or more high temperature.The good permeability of silicon rubber, OTR oxygen transmission rate are highest in synthetic polymer.In addition, silicon rubber is also
It with physiological inertia, not will lead to the prominent characteristic of blood coagulation, therefore be widely used in medical field.
However, traditional silicon rubber is difficult to meet special demand, and as science and technology is constantly progressive, to the function of silicon rubber
Change demand is continuously increased, including mechanics enhances, is fire-retardant, sterilizing, close and distant aquation is modified etc..For example, patent of invention
CN201610077691.4 has invented a kind of preparation method of silastic surface hydrophilic coating, and hydrophilic coating has good attachment
Power and biocompatibility, especially suitable for field of biomedical materials；Patent of invention CN201510644904.2 passes through antibacterial
Ion is attached on White Carbon black carrier, has obtained a kind of antibacterial high temperature silicone rubber；Patent CN201610146685.X uses multilayer
Structure design is prepared for a kind of super soft organosilicon leather, extends the use scope of organosilicon leather；For another example patent
CN201510932418.0, which is disclosed, has invented a kind of multi-component silicon rubber, has antistatic and flame retarding function；Patent
CN201310285809.9 is prepared for a kind of transparent silicone rubber containing ladder-like polysiloxane, has both improved the machinery of silicon rubber
Mechanical property, and improve the heat resistance and radiation resistance of silicon rubber.It can be seen that can by structure design and composite algorithm
To realize the functionalization of silicon rubber, however, often demand material therefor has multiple performance for extraordinary application field, such as
While meeting mechanical strength, the multiple performances such as heat-resisting, fast light may be also needed to meet.And the material obtained by composite algorithm,
It will cause pollution in the processes such as use process, failure and degradation and limit its extensive use.Still further aspect is removed
Properties mentioned above is expected to further develop the huge applications of silicon rubber if be able to achieve continuous poriferousization of silicon rubber
Potentiality, such as porous silicone rubber can be used as cell culturing bracket, drug and catalyst carrier, in addition, having by microwell plate effect
It hopes and realizes super sound-insulating and heat-insulating.Although being able to achieve continuous Jie of above functions however, there is the report of foam rubber and macropore rubber
Hole rubber is rare.
Summary of the invention
In view of the deficiencies of the prior art with the limitation of material property, it is a primary object of the present invention to by structure design and
Preparation method innovation, prepares transparent meso silicon elastomeric precursor, that is, uses sol-gel chemistry, realizes that bi-component, original position are mild and hands over
Join sulfidation, most afterwards through supercritical fluid drying or freeze-drying obtain transparency it is adjustable, with continuous mesoporous silicon elasticity
Precursor.The transparency of the transparent meso silicon elastomeric precursor is from 50%-80%, density 300g/m3-700g/m3, elasticity modulus from
1MPa-20MPa etc., in addition, the transparent meso silicon elastomeric precursor has excellent bio-compatibility, continuous porous structure,
Specific surface area is up to 100m2/ g is with a wide range of applications in industries such as special type protection, industry, transport, food and drink, medicine.
To realize aforementioned invention purpose, The technical solution adopted by the invention is as follows:
A kind of transparent meso silicon elastomeric precursor is passed through using hydroxyl-terminated injecting two methyl siloxane and organosiloxane as raw material
Sol-gel chemistry changes to form gel after, obtained through special drying process a kind of transparency it is high, with continuous mesoporous saturating
Bright mesoporous silicon elastomeric precursor；The transparency of the transparent meso silicon elastomeric precursor is 50%-80%, density 300g/m3-
700g/m3, elasticity modulus 1MPa-20MPa, specific surface area is up to 100m2/g。
Further, the stoichiometric ratio (molal quantity ratio) of the hydroxyl-terminated injecting two methyl siloxane and organosiloxane
For 1:1 to 1:5.And it is without being limited thereto.
Further, the number-average molecular weight of the hydroxyl-terminated injecting two methyl siloxane is 350-1000, and without being limited thereto.
Further, the siloxanes include tetramethoxy siloxanes, ethyl orthosilicate, or any combination thereof.
The present invention also provides a kind of preparation methods of transparent meso silicon elastomeric precursor, include the following steps:
(1) a certain amount of hydroxyl-terminated injecting two methyl siloxane and organosiloxane are sufficiently mixed a certain amount of organic molten
In agent, stirring is to sufficiently dissolving and form homogeneous mixed liquor；
(2) the homogeneous mixed liquor is added in a certain amount of catalyst, stands form Silica hydrogel after mixing evenly；
(3) Silica hydrogel is washed into removal catalyst, unreacted monomer etc., is most obtained afterwards through special drying process
Bright mesoporous silicon elastomeric precursor.
As more one of preferred embodiment, step (1) is specifically included: by a certain amount of terminal hydroxy group poly dimethyl silicon
Oxygen alkane and organosiloxane are sufficiently mixed in a certain amount of solvent, and stirring is to sufficiently dissolving and form homogeneous mixed liquor.
Further, the number-average molecular weight of the hydroxyl-terminated injecting two methyl siloxane is 350-1000, and without being limited thereto.
Further, the siloxanes include tetramethoxy siloxanes, ethyl orthosilicate, or any combination thereof.
Further, the solvent include: methanol, ethyl alcohol, tetrahydrofuran, n,N-Dimethylformamide, dimethyl sulfoxide,
N-Methyl pyrrolidone and both the above or a variety of any combination.
Further, the stoichiometric ratio of the hydroxyl-terminated injecting two methyl siloxane and organosiloxane are as follows: the two is rubbed
Your quantity ratio is 1:1 to 1:5.
Further, the solvent usage is 1 to 10 times of total mass of raw material.
As more one of preferred embodiment, step (2) is specifically included: a certain amount of catalyst being added above-mentioned equal
Liquid is mixed, stands form Silica hydrogel after mixing evenly.
Further, the catalyst includes ammonium hydroxide, ammonium chloride, urea, triethylamine, sodium hydroxide, potassium hydroxide, pyrrole
Pyridine or both the above or a variety of any combination.
Further, the dosage of the catalyst is the 5% to 10% of material quality score.
As more one of preferred embodiment, step (3) specifically include by the Silica hydrogel wash removal catalyst,
Most transparent meso silicon elastomeric precursor is prepared through supercritical drying afterwards in unreacted monomer etc..
Further, washing includes following parameter: solvent and the gel dispersion liquid phase for washing use are same；Wash time is greater than
6 hours.
Further, washing times are greater than 2 times.
Further, wash temperature is boiling point of the room temperature to solvent for use.
Further, the drying means includes supercritical fluid drying, freeze-drying.
Further, drying time is no less than 5 hours.
Detailed description of the invention
Fig. 1 is synthetic route schematic diagram of the present invention.
Fig. 2 is chemical equation schematic diagram of the present invention.
Fig. 3 is transparent meso silicon elastomeric precursor stereoscan photograph figure prepared by the embodiment of the present invention 1.
Fig. 4 is transparent meso silicon elastomeric precursor stereoscan photograph figure prepared by the embodiment of the present invention 2.
Fig. 5 is transparent meso silicon elastomeric precursor stereoscan photograph figure prepared by the embodiment of the present invention 3.
Fig. 6 is transparent meso silicon elastomeric precursor stereoscan photograph figure prepared by the embodiment of the present invention 4.
Fig. 7 is transparent meso silicon elastomeric precursor stereoscan photograph figure prepared by the embodiment of the present invention 5.
Fig. 8 is transparent meso silicon elastomeric precursor stereoscan photograph figure prepared by the embodiment of the present invention 6.
Specific embodiment
In view of the deficiency in the prior art and system, inventor is studied for a long period of time and is largely practiced, and proposes this hair
Bright mentality of designing and scheme passes through colloidal sol-mainly using hydroxyl-terminated injecting two methyl siloxane and organosiloxane as raw material
Gel chemistries method prepares gel, and then the gel is washed, is most prepared afterwards through supercritical drying or freeze-drying transparent
Mesoporous silicon elastomeric precursor.
Therefore, a kind of transparent meso silicon elastomeric precursor of the present invention, with hydroxyl-terminated injecting two methyl siloxane and organosiloxane
For raw material, after sol-gel chemistry changes and to form gel, obtain that a kind of transparency is high, has through special drying process
Continuous mesoporous transparent meso silicon elastomeric precursor；The transparency of the transparent meso silicon elastomeric precursor is 50%-80%, and density is
300g/m3-700g/m3, elasticity modulus 1MPa-20MPa, specific surface area is up to 100m2/g。
Further, the stoichiometric ratio (molal quantity ratio) of the hydroxyl-terminated injecting two methyl siloxane and organosiloxane
For 1:1 to 1:5.And it is without being limited thereto.
Further, the number-average molecular weight of the hydroxyl-terminated injecting two methyl siloxane is 350-1000, and without being limited thereto.
Further, the siloxanes include tetramethoxy siloxanes, ethyl orthosilicate, or any combination thereof.
The present invention also provides a kind of preparation methods of transparent meso silicon elastomeric precursor, include the following steps:
(1) a certain amount of hydroxyl-terminated injecting two methyl siloxane and organosiloxane are sufficiently mixed a certain amount of organic molten
In agent, stirring is to sufficiently dissolving and form homogeneous mixed liquor；
(2) the homogeneous mixed liquor is added in a certain amount of catalyst, stands form Silica hydrogel after mixing evenly；
(3) Silica hydrogel is washed into removal catalyst, unreacted monomer etc., is most obtained afterwards through special drying process
Bright mesoporous silicon elastomeric precursor.
As more one of preferred embodiment, step (1) is specifically included: by a certain amount of terminal hydroxy group poly dimethyl silicon
Oxygen alkane and organosiloxane are sufficiently mixed in a certain amount of solvent, and stirring is to sufficiently dissolving and form homogeneous mixed liquor.
Further, the number-average molecular weight of the hydroxyl-terminated injecting two methyl siloxane is 350-1000, and without being limited thereto.
Further, the siloxanes include tetramethoxy siloxanes, ethyl orthosilicate, or any combination thereof.
Further, the solvent include: methanol, ethyl alcohol, tetrahydrofuran, n,N-Dimethylformamide, dimethyl sulfoxide,
N-Methyl pyrrolidone and both the above or a variety of any combination.
Further, the stoichiometric ratio of the hydroxyl-terminated injecting two methyl siloxane and organosiloxane are as follows: the two is rubbed
Your quantity ratio is 1:1 to 1:5.
Further, the solvent usage is 1 to 10 times of total mass of raw material.
As more one of preferred embodiment, step (2) is specifically included: a certain amount of catalyst being added described equal
Liquid is mixed, stands form gel after mixing evenly.
Further, the catalyst includes ammonium hydroxide, ammonium chloride, urea, triethylamine, sodium hydroxide, potassium hydroxide, pyrrole
Pyridine or both the above or a variety of any combination.
Further, the dosage of the catalyst is the 5% to 10% of material quality score.
As more one of preferred embodiment, step (3) specifically include by the Silica hydrogel wash removal catalyst,
Most transparent meso silicon elastomeric precursor is prepared through supercritical drying afterwards in unreacted monomer etc..
Further, washing includes following parameter: solvent and the gel dispersion liquid phase for washing use are same；Wash time is greater than
6 hours.
Further, washing times are greater than 2 times.
Further, wash temperature is boiling point of the room temperature to solvent for use.
Further, the drying means includes supercritical fluid drying, freeze-drying.
Further, drying time is no less than 5 hours.Below in conjunction with several examples and drawings to technical side of the invention
Case is further explained.
Embodiment 1
(1) the mixed liquor preparation of raw material: taking 50 parts of molecular weight is 350 hydroxyl-terminated injecting two methyl siloxane, and 50 parts of R are first
The siloxanes of base, i.e. tetramethoxy-silicane are substantially dissolved in 100 parts of dehydrated alcohols, after stirring 5 hours, obtain uniform colorless
Mixed solution.
(2) gelation process: 10 parts of concentrated ammonia liquor is slowly dropped into above-mentioned mixed liquor, after stirring 1 hour, solution transfer
It into closed container, and is statically placed in 80 DEG C of environment, forms colorless transparent gel after 24 hours.
(3) washing and drying: above-mentioned clear gel is placed in 100 parts of dehydrated alcohols, and it is small that 12 are stirred under the conditions of 50 DEG C
When, it is washed 2 times with clean dehydrated alcohol by the same terms again later.It is most dry through Supercritical Ethanol afterwards, obtain transparent meso
Silicon elastomeric precursor.The preparation method and reaction equation of the transparent meso silicon elastomeric precursor are shown in Fig. 1 and Fig. 2, scanning electron microscope respectively
Figure is shown in Fig. 3, other physical parameters such as density, light transmittance, Young's modulus, specific surface area etc. refer to table 1.
Embodiment 2
(1) the mixed liquor preparation of raw material: taking 50 parts of molecular weight is 1000 hydroxyl-terminated injecting two methyl siloxane, and 250 parts of R are
The siloxanes of ethyoxyl, i.e. ethyl orthosilicate are substantially dissolved in 300 parts of anhydrous methanols, after stirring 10 hours, obtain uniform nothing
The mixed solution of color.
(2) gelation process: 15 parts of concentrated ammonia liquor is slowly dropped into above-mentioned mixed liquor, after stirring 2 hours, solution transfer
It into closed container, and is statically placed in 50 DEG C of environment, forms colorless transparent gel after 8 hours.
(3) washing and drying: above-mentioned clear gel is placed in 300 parts of anhydrous methanols, and it is small that 12 are stirred under the conditions of 60 DEG C
When, it is washed 1 time with clean anhydrous methanol by the same terms again later.Most transparent Jie is dried to obtain through supercritical carbon dioxide afterwards
Hole silicon elastomeric precursor.The preparation method and reaction equation of the transparent meso silicon elastomeric precursor are shown in Fig. 1 and Fig. 2, scanning electricity respectively
Mirror figure is shown in Fig. 4, other physical parameters such as density, light transmittance, Young's modulus, specific surface area etc. refer to table 1.
Embodiment 3
(1) the mixed liquor preparation of raw material: taking 50 parts of molecular weight is 550 hydroxyl-terminated injecting two methyl siloxane, and 100 parts of R are
The siloxanes of ethyoxyl, i.e. ethyl orthosilicate are substantially dissolved in 400 parts of tetrahydrofurans, after stirring 8 hours, obtain uniform nothing
The mixed solution of color.
(2) gelation process: 8 parts of concentrated ammonia liquor is slowly dropped into above-mentioned mixed liquor, after stirring 2 hours, solution transfer
It into closed container, and is statically placed in 60 DEG C of environment, forms colorless transparent gel after 48 hours.
(3) washing and drying: above-mentioned clear gel is placed in 500 parts of dehydrated alcohols, and it is small that 12 are stirred under the conditions of 60 DEG C
When, it is washed 2 times, is replaced 5 times through water again later, displacement one in every 10 hours by the same terms with clean dehydrated alcohol again later
It is secondary.It is finally freeze-dried to obtain transparent meso silicon elastomeric precursor.The preparation method and reaction of the transparent meso silicon elastomeric precursor
Equation is shown in that Fig. 1 and Fig. 2, scanning electron microscope (SEM) photograph are shown in Fig. 5 respectively, other physical parameters such as density, Young's modulus, compares table at light transmittance
Area etc. refers to table 1.
Embodiment 4
(1) the mixed liquor preparation of raw material: taking 50 parts of molecular weight is 650 hydroxyl-terminated injecting two methyl siloxane, and 150 parts of R are
The siloxanes of ethyoxyl, i.e. ethyl orthosilicate are substantially dissolved in 150 parts of DMF, after stirring 8 hours, obtain the mixed of uniform colorless
Close solution.
(2) gelation process: 20 parts of concentrated ammonia liquor is slowly dropped into above-mentioned mixed liquor, after stirring 2 hours, solution transfer
It into closed container, and is statically placed in 100 DEG C of environment, forms colorless transparent gel after 18 hours.
(3) washing and drying: above-mentioned clear gel is placed in 300 parts of dehydrated alcohols, and it is small that 12 are stirred under the conditions of 60 DEG C
When, it is washed 2 times with clean dehydrated alcohol by the same terms again later.Most transparent Jie is dried to obtain through supercritical carbon dioxide afterwards
Hole silicon elastomeric precursor.The preparation method and reaction equation of the transparent meso silicon elastomeric precursor are shown in Fig. 1 and Fig. 2, scanning electricity respectively
Mirror figure is shown in Fig. 6, other physical parameters such as density, light transmittance, Young's modulus, specific surface area etc. refer to table 1.
Embodiment 5
(1) the mixed liquor preparation of raw material: taking 50 parts of molecular weight is 750 hydroxyl-terminated injecting two methyl siloxane, and 200 parts of R are
The siloxanes of ethyoxyl, i.e. ethyl orthosilicate are substantially dissolved in 250 parts of DMSO, after stirring 8 hours, obtain uniform colorless
Mixed solution.
(2) gelation process: 5 parts of concentrated ammonia liquor is slowly dropped into above-mentioned mixed liquor, after stirring 8 hours, solution transfer
It into closed container, and is statically placed in 120 DEG C of environment, forms colorless transparent gel after 24 hours.
(3) washing and drying: above-mentioned clear gel is placed in 500 parts of dehydrated alcohols, and it is small that 12 are stirred under the conditions of 60 DEG C
When, it is washed 2 times with clean dehydrated alcohol by the same terms again later.Most transparent meso silicon elasticity is obtained through Supercritical Ethanol afterwards
Precursor.The preparation method and reaction equation of the transparent meso silicon elastomeric precursor are shown in that Fig. 1 and Fig. 2, scanning electron microscope (SEM) photograph are shown in figure respectively
7, other physical parameters such as density, light transmittance, Young's modulus, specific surface area etc. refer to table 1.
Embodiment 6
(1) the mixed liquor preparation of raw material: taking 50 parts of molecular weight is 850 hydroxyl-terminated injecting two methyl siloxane, and 100 parts of R are
The siloxanes of ethyoxyl, i.e. ethyl orthosilicate are substantially dissolved in 200 parts of ethyl alcohol, after stirring 8 hours, obtain uniform colorless
Mixed solution.
(2) gelation process: 5 parts of concentrated ammonia liquor is slowly dropped into above-mentioned mixed liquor, after stirring 8 hours, solution transfer
It into closed container, and is statically placed in 60 DEG C of environment, forms colorless transparent gel after 24 hours.
(3) washing and drying: above-mentioned clear gel is placed in 200 parts of dehydrated alcohols, and it is small that 12 are stirred under the conditions of 60 DEG C
When, it is washed 2 times with clean dehydrated alcohol by the same terms again later.It is most dry through supercritical carbon dioxide afterwards, it obtains transparent
Mesoporous silicon elastomeric precursor.The preparation method and reaction equation of the transparent meso silicon elastomeric precursor are shown in Fig. 1 and Fig. 2 respectively, scanning
Electron microscope is shown in Fig. 8, other physical parameters such as density, light transmittance, Young's modulus, specific surface area etc. refer to table 1.
The performance parameter of obtained transparent meso silicon elastomeric precursor in 1 embodiment 1-6 of table
The foregoing examples are merely illustrative of the technical concept and features of the invention, its object is to allow the person skilled in the art to be
It cans understand the content of the present invention and implement it accordingly, it is not intended to limit the scope of the present invention.It is all smart according to the present invention
The equivalent transformation or modification that refreshing essence is done, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of transparent meso silicon elastomeric precursor, it is characterised in that with hydroxyl-terminated injecting two methyl siloxane and organosiloxane be original
Material, after sol-gel chemistry changes and to form gel, a kind of transparency obtained through special drying process is high, has company
Continue mesoporous transparent meso silicon elastomeric precursor；The transparency of the transparent meso silicon elastomeric precursor is 50%-80%, and density is
300g/m3-700g/m3, elasticity modulus 1MPa-20MPa, specific surface area is up to 100m2/g。
2. transparent meso silicon elastomeric precursor according to claim 1, which is characterized in that the terminal hydroxy group polydimethylsiloxanes
The stoichiometric ratio (molal quantity ratio) of alkane and organosiloxane is 1:1 to 1:5.
3. transparent meso silicon elastomeric precursor according to claim 1, which is characterized in that the terminal hydroxy group polydimethylsiloxanes
The number-average molecular weight of alkane is 350-1000.
4. transparent meso silicon elastomeric precursor according to claim 1, which is characterized in that the organosiloxane includes tetramethyl
Oxygroup siloxanes, ethyl orthosilicate, or any combination thereof.
5. a kind of preparation method of transparent meso silicon elastomeric precursor according to claim 1, it is characterised in that the preparation
Method includes the following steps:
(1) a certain amount of hydroxyl-terminated injecting two methyl siloxane and organosiloxane are sufficiently mixed in a certain amount of organic solvent
In, stirring is to sufficiently dissolving and form homogeneous mixed liquor；
(2) the homogeneous mixed liquor is added in a certain amount of catalyst, stands form Silica hydrogel after mixing evenly；
(3) Silica hydrogel is washed into removal catalyst, unreacted monomer etc., most obtains transparent Jie through special drying process afterwards
Hole silicon elastomeric precursor.
6. preparation method according to claim 5, it is characterised in that: step (1) described solvent includes: methanol, ethyl alcohol, four
Hydrogen furans, N,N-dimethylformamide, dimethyl sulfoxide, N-Methyl pyrrolidone or both the above or a variety of any combination.
7. preparation method according to claim 5 or 6, it is characterised in that: step (1) solvent usage is the total matter of raw material
1 to 10 times of amount.
8. preparation method according to claim 5, it is characterised in that: step (2) described catalyst includes ammonium hydroxide, chlorination
Ammonium, urea, triethylamine, sodium hydroxide, potassium hydroxide, pyridine or both the above or a variety of any combination；And/or it described urges
The dosage of agent is the 5% to 10% of material quality score.
9. preparation method according to claim 5, it is characterised in that: step (3) washing includes following parameter: washing
The solvent of use and gel dispersion liquid phase are same；And/or wash time is greater than 6 hours；And/or washing times are greater than 2 times；And/or
Wash temperature is boiling temperature of the room temperature to solvent for use.
10. preparation method according to claim 5, it is characterised in that: step (3) described drying means includes shooting flow
Body seasoning or freeze-drying；And/or the supercritical fluid drying includes Supercritical Ethanol, supercritical methanol, surpasses and face
Boundary's carbon dioxide, and it is without being limited thereto；And/or the freeze-drying condition are as follows: condenser temperature is-45-60 DEG C, and vacuum pressure is small
In 500Pa.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103525358A (en) * | 2013-07-09 | 2014-01-22 | 杭州师范大学 | Preparation method and application of transparent silicon rubber containing trapezoidal polysilsesquioxane |
| CN104071796A (en) * | 2013-03-28 | 2014-10-01 | 北京化工大学 | Preparation method of flexible silicon dioxide aerosol |
| CN108117082A (en) * | 2017-12-27 | 2018-06-05 | 武汉理工大学 | A kind of siloxanes toughening modifying SiO2Aeroge and preparation method thereof |
-
2019
- 2019-08-19 CN CN201910763078.1A patent/CN110452409A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104071796A (en) * | 2013-03-28 | 2014-10-01 | 北京化工大学 | Preparation method of flexible silicon dioxide aerosol |
| CN103525358A (en) * | 2013-07-09 | 2014-01-22 | 杭州师范大学 | Preparation method and application of transparent silicon rubber containing trapezoidal polysilsesquioxane |
| CN108117082A (en) * | 2017-12-27 | 2018-06-05 | 武汉理工大学 | A kind of siloxanes toughening modifying SiO2Aeroge and preparation method thereof |
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Application publication date: 20191115 |