CN109666149A - A kind of preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure - Google Patents
A kind of preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure Download PDFInfo
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Abstract
The present invention relates to graphene-based silicone materials technical fields, a kind of preparation method of graphene-based polysiloxanes of silicon oxygen six-membered ring structure is provided, using graphene oxide as raw material, it is reacted using sol-gal process with silane coupler modified polysiloxanes after silane coupler modified, the graphene-based polysiloxanes of silicon oxygen six-membered ring structure is made, effectively promote dispersion stabilization of the graphene oxide in polysiloxanes, polysiloxanes and graphene are had complementary advantages, it provides a kind of with electrostatic screen, physical property is high, mechanical strength is strong, the water-soluble graphene modified polyorganosiloxane material of the excellent properties such as color inhibition.
Description
Technical field
The present invention relates to graphene-based silicone materials technical field, in particular to a kind of silicon oxygen six-membered ring structure graphite
The preparation method of alkenyl polysiloxanes.
Background technique
Polysiloxanes has many excellent performances because of its unique structure, is widely used in electronic apparatus, automobile is handed over
The numerous areas such as logical, chemical industry, light industry, machinery, building, fiber.Polysiloxanes is a kind of with different viscositys, nontoxic, odorless, nothing
The nonflammable liquid grease of burn into, have viscosity-temperature coefficient is small, high-low temperature resistant, anti-oxidant, flash-point is high, volatility is small, it is nontoxic
Etc. characteristics.But polysiloxane hydrophobic is stronger, there is the phenomenon that demulsification, roll banding in product use process, it is furthermore traditional poly-
Siloxanes also has xanthochromia, increases the defects of product hydrophobicity.Therefore, how to introduce in polysiloxane structure has highizationer
Learn activity, and the polymer architecture that can be effectively combined with product, so that polysiloxanes can be very good anchor in product surface and real
Now hydrophilic is the main problem that polysiloxanes applies required solution.
Currently in order to aforementioned technical problem is solved, and it is existing that graphene/polysiloxanes composite material is studied, using object
Reason blending method mixes graphene or graphene oxide with polysiloxanes, and graphene is the highest two-dimensional nano of nature intensity
Material has extraordinary toughness, can be used as nano-filled object, for enhancing, toughening polymer material；Graphene oxide is stone
The derivative of black alkene is a kind of flexible material of non-traditional kenel, the spy with polymer, colloid, film and amphiphatic molecule
Property, therefore graphene or graphene oxide and polysiloxanes is compound, physical property, the machinery that can improve composite material are strong
Degree, while the performances such as composite material color inhibition, water solubility are assigned, it is asked with solving existing silicone materials using existing technology
Topic.
But graphene or graphene oxide are carried out using physical blending process and mixed with polysiloxanes, can in the presence of just like
Lower problem: (1) there are the technological deficiencies such as easy to reunite, reactionlessness for graphene, accordingly, it is difficult to which graphene to be directly dispersed into polymerization
In objects system, being difficult to the active force to its functional modification, between graphene and polysiloxanes using graphene, there is only van
Der walls power, to the physical and chemical performance of material without being obviously improved；And relative to graphene, though graphene oxide can preferably divide
Be dispersed in polymeric system, but since its two-dimensional structure has been destroyed, thus on physical and chemical performance opposite graphene be mixed with it is bright
Aobvious decline；(2) compound mixing is carried out using physical blending process, is logical between graphene or graphene oxide and polysiloxanes
Cross van der walls power and realize mixed binding, and polysiloxane backbone is all made of singly-bound, Si-O singly-bound for flexibility most
Good singly-bound, therefore the barrier potential Δ μ b changed between polysiloxanes space conformation is much smaller than outer field action energy, therefore silicone monomers
It is randomly curled in Coiling-type in space, and polysiloxanes segment can constantly change its conformation.Much due to intermolecular force
It is weaker than covalent bonding, polysiloxanes segment flexibility is too strong, relies on van der walls power and is difficult to graphene or oxidation
The good anchor of graphene causes graphene or the graphene oxide dispersibility in polysiloxanes excessively weak on polysiloxanes, right
Physical and chemical performance promotion is relatively limited, and precipitating easy to form or suspension, greatly reduces the comprehensive performance of composite material, practical
Property is low.
Summary of the invention
Therefore, for above-mentioned problem, the present invention proposes a kind of system of graphene-based polysiloxanes of silicon oxygen six-membered ring structure
Preparation Method is gathered using sol-gal process with silane coupler modified after silane coupler modified using graphene oxide as raw material
Siloxane reactions, are made the graphene-based polysiloxanes of silicon oxygen six-membered ring structure, effectively promote graphene oxide in polysiloxanes
Dispersion stabilization, polysiloxanes and graphene are had complementary advantages, providing a kind of has that electrostatic screen, physical property be high, machine
The water-soluble graphene modified polyorganosiloxane material of the excellent properties such as the strong, color inhibition of tool intensity.
To realize above-mentioned technical problem, the solution that the present invention takes are as follows: a kind of silicon oxygen six-membered ring structure is graphene-based
The preparation method of polysiloxanes, includes the following steps:
Step (1) graphene oxide is modified: adding graphene oxide into silane coupling agent, N, bis- ring of N- is then added
Hexyl carbodiimide, ultrasonic disperse 20-200min, obtains graphene oxide dispersion, is transferred in reactor at 50-100 DEG C
12-72h is reacted, reaction mixture is dried in vacuo to obtain solid powder through filtration washing, obtains modified oxidized stone after carrying out reduction
Black alkene；
Step (2) modified polyorganosiloxane preparation: by siloxanyl monomers, silane coupling agent, end-capping reagent, catalyst, crosslinking agent
3-8h is reacted at 70-140 DEG C, obtains modified polyorganosiloxane；
The graphene-based polysiloxanes preparation of step (3) silicon oxygen six-membered ring structure: deionization is added in modified graphene oxide
In water, ultrasonic disperse 20-200min obtains modified graphene oxide dispersion liquid；Modified oxidized stone is added in modified polyorganosiloxane
In black alkene dispersion liquid, triethylamine is added, colloidal sol is made in 3-8h under 10-50 DEG C of reaction, is then warming up to 60-100 DEG C of reaction
Gel solution is made in 1-5h；Gel is obtained after gel solution is dried in vacuo, then obtains silicon oxygen hexatomic ring knot after carrying out reduction
The graphene-based silicone materials of structure.
Wherein, silane coupling agent described in step (1) is at least 3- chloropropyl triethoxysilane, three ethoxy of 3- aminopropyl
One of base silane, 3- (2,3 the third oxygen of epoxy) propyl-triethoxysilicane, triethoxysilane.
Wherein, concentration of the graphene oxide in silane coupling agent described in step (1) is 1-15g/L, the catalyst
Concentration in silane coupling agent is 1-15g/L.
Wherein, siloxanyl monomers described in step (2) are octamethylcy-clotetrasiloxane.
Wherein, silane coupling agent described in step (2) is at least 3- chloropropyl triethoxysilane, three ethoxy of 3- aminopropyl
One of base silane, 3- (2,3 the third oxygen of epoxy) propyl-triethoxysilicane, triethoxysilane.
Wherein, end-capping reagent described in step (2) is at least 1,3- bis- (3- glycydoxy) -1,1,3,3- tetra-
One of tetramethyldisiloxane, hexamethyldisiloxane.
Wherein, catalyst described in step (2) is at least potassium hydroxide, lithium hydroxide, one in tetramethylammonium hydroxide
Kind.
Wherein, crosslinking agent described in step (2) is at least one of epoxy prapanol, third chlorine of epoxy.
Wherein, the concentration of silane coupling agent described in step (2) is 0.1-5%, and the end-capping reagent concentration is 0.1-
1%, the catalyst concn is 0.01-0.2%, and the crosslinker concentration is 0-4%.
Wherein, the concentration of modified graphene oxide in deionized water described in step (3) is 0.5-10g/L；It is described to change
Property concentration of the polysiloxanes in modified graphene oxide dispersion liquid be 100-1000g/L, the triethylamine is modified oxidized
Concentration in graphene dispersing solution is 0.005-0.025g/L.
Wherein, the ultrasonic wave dispersion power of ultrasonic disperse described in step (1) step (3) is 50-600W.
Wherein, vacuum drying temperature described in step (1) step (3) is 30-80 DEG C, drying time 12-72h.
Wherein, restoring method described in step (1) step (3), which is at least, uses 0.5-5% liquor kalii iodide reduction treatment
3-24h, using 0.5-5% hydrazine hydrate solution reduction treatment 3-24h, at 50-150 DEG C in reduction treatment 30-90min one
Kind.
By using preceding solution, the beneficial effects of the present invention are: the silicon oxygen six-membered ring structure is graphene-based poly-
The preparation method of siloxanes has the advantage that compared with the existing technology
(1) using after graphene oxide covalent bond functional modification and as active site, chemical graft polysiloxanes.
It is steady not only to can be further improved dispersion of its lamella in all kinds of solvents, polymer by the graphene oxide of functional modification
It is qualitative, and graphene oxide after covalent bond functional modification introduce function chemoattractant molecule, polymer, group after can be significant
The compatibility for improving graphene oxide and polymer, so that graphene oxide can be in matrixes such as function chemoattractant molecule, polymer
In more preferable, dispersion more evenly.
(2) use chemical graft process graft polysiloxane on graphene oxide, by chemical bond by graphene oxide and
Polysiloxanes bonding, so that graphene oxide is uniformly dispersed in polysiloxanes, the active site on simultaneous oxidation graphene
So that polysiloxanes branching to a certain extent, hinders the interior rotation of chain, and by the active group of silane coupling agent introducing, make
It obtains and is able to form the intermolecular forces such as conjugatedπbond, hydrogen bond between polysiloxanes and graphene oxide, further promote oxidation stone
Dispersion stabilization of the black alkene in polysiloxanes.
(3) modified graphene oxide is restored, so that graphene oxide is restored the structure of script graphene, is only side
There are still a small amount of oxygen-containing functional group, this method to obtain good dispersion effect while promoting its physical and chemical performance edge.
Therefore, by the preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure, oxidation stone is effectively promoted
Dispersion stabilization of the black alkene in polysiloxanes realizes the effective compound of graphene oxide and polysiloxanes, effectively by poly- silicon oxygen
Alkane and graphene have complementary advantages, and providing a kind of has that certain conductive capability, physical property are high, mechanical strength is strong, color inhibition, make
With the water-soluble graphene modified polyorganosiloxane material of the excellent properties such as service life length.
Specific embodiment
The present invention is specifically described below by specific embodiment, whereby to the present invention how applied technology method
Technical problem is solved, and the realization process for reaching technical effect can fully understand and implement, it is necessary to indicated herein
It is that the present embodiment is served only for that invention is further explained, should not be understood as limiting the scope of the invention, the neck
The person skilled in the art in domain can make some nonessential modifications and adaptations according to the content of aforementioned present invention.
Unless otherwise specified, the conventional hand that technological means employed in embodiment is well known to those skilled in the art
Section, used reagent and product are also available commercial.The various processes and method being not described in detail are in this field
Well known conventional method, the source of agents useful for same, trade name and it is necessary to list its constituent person, on the first appearance
It indicates.
Embodiment 1
A kind of preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure, comprising the following steps:
Step (1) graphene oxide is modified: graphene oxide (single-layer graphene oxide) is added to silane coupling agent (3-
Aminopropyl triethoxysilane) in, N is then added, N- dicyclohexylcarbodiimide, the graphene oxide is in silane coupling agent
In concentration be 5g/L, the N, concentration of the N- dicyclohexylcarbodiimide in silane coupling agent be 5g/L, ultrasonic disperse
60min (it is 120W that ultrasonic wave, which disperses power), obtains graphene oxide dispersion, is transferred in reactor and reacts for 24 hours at 70 DEG C,
Reaction mixture is obtained into solid powder through filtration washing vacuum drying (vacuum drying temperature is 50 DEG C, drying time 48h),
Modified graphene oxide is obtained after being restored (restoring method is using 2% liquor kalii iodide reduction treatment 6h)；
Step (2) modified polyorganosiloxane preparation: by siloxanyl monomers (octamethylcy-clotetrasiloxane), silane coupling agent (3-
Aminopropyl triethoxysilane), end-capping reagent (hexamethyldisiloxane), catalyst (potassium hydroxide), crosslinking agent (epoxy prapanol)
4h is reacted at 110 DEG C, obtains modified polyorganosiloxane；Wherein, the silane coupling agent concentration is 2%, and the end-capping reagent is dense
Degree is 0.4%, and the catalyst concn is 0.06%, and the crosslinker concentration is 1%；
The graphene-based polysiloxanes preparation of step (3) silicon oxygen six-membered ring structure: deionization is added in modified graphene oxide
In water, the concentration of modified graphene oxide in deionized water is 2g/L, and (ultrasonic wave disperses power to ultrasonic disperse 60min
120W), modified graphene oxide dispersion liquid is obtained；Modified polyorganosiloxane is added in modified graphene oxide dispersion liquid, it is modified
Concentration of the polysiloxanes in modified graphene oxide dispersion liquid is 400g/L, adds triethylamine, the triethylamine is in modification
Concentration in graphene oxide dispersion is 0.015g/L, and colloidal sol is made in 5h under 30 DEG C of reactions, is then warming up to 70 DEG C of reactions
Gel solution is made in 3h, will obtain after gel solution vacuum drying (vacuum drying temperature is 50 DEG C, drying time 48h)
Gel, then that silicon oxygen six-membered ring structure is obtained after being restored (restoring method be at 100 DEG C reduction treatment 60min) is graphene-based poly-
Siloxanes.
Embodiment 2
A kind of preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure, includes the following steps:
Step (1) graphene oxide is modified: graphene oxide (single-layer graphene oxide) is added to silane coupling agent (3-
Chloropropyl triethoxysilane) in, concentration of the graphene oxide in silane coupling agent is 7.5g/L, and N, bis- ring of N- is then added
Hexyl carbodiimide, the N, concentration of the N- dicyclohexylcarbodiimide in silane coupling agent are 7.5g/L, ultrasonic disperse
90min (it is 60W that ultrasonic wave, which disperses power), obtains graphene oxide dispersion, is transferred in reactor and reacts 36h at 70 DEG C,
Reaction mixture is obtained into solid powder through filtration washing vacuum drying (vacuum drying temperature is 35 DEG C, drying time 60h),
Restored again (restoring method be obtain modified graphene oxide after 2.5% hydrazine hydrate solution reduction treatment 8h)；
Step (2) modified polyorganosiloxane preparation: by siloxanyl monomers (octamethylcy-clotetrasiloxane), silane coupling agent (3-
Aminopropyl triethoxysilane), end-capping reagent (two silicon oxygen of 1,3- bis- (3- glycydoxy) -1,1,3,3- tetramethyl
Alkane), catalyst (tetramethylammonium hydroxide) react 6h at 90 DEG C, obtain modified polyorganosiloxane；Wherein, the silane coupling agent
Concentration is 2%, and the end-capping reagent concentration is 0.8%, and the catalyst concn is 0.06%；
The graphene-based polysiloxanes preparation of step (3) silicon oxygen six-membered ring structure: deionization is added in modified graphene oxide
In water, the concentration of modified graphene oxide in deionized water is 2g/L, and (ultrasonic wave disperses power to ultrasonic disperse 90min
60W), modified graphene oxide dispersion liquid is obtained；Modified polyorganosiloxane is added in modified graphene oxide dispersion liquid, it is modified poly-
Concentration of the siloxanes in modified graphene oxide dispersion liquid is 350g/L, adds triethylamine, triethylamine is in modified oxidized stone
Concentration in black alkene dispersion liquid is 0.02g/L, and colloidal sol is made in 3h under 25 DEG C of reactions, is then warming up to 80 DEG C of reaction 3h and is made solidifying
Glue solution will obtain gel after gel solution vacuum drying (vacuum drying temperature is 35 DEG C, drying time 60h), then
It is graphene-based poly- that silicon oxygen six-membered ring structure is obtained after being restored (restoring method is using 2.5% hydrazine hydrate solution reduction treatment 8h)
Siloxanes.
Embodiment 3
A kind of preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure, includes the following steps:
Step (1) graphene oxide is modified: graphene oxide (two layers of graphene oxide) is added to silane coupling agent (3-
(2,3 the third oxygen of epoxy) propyl-triethoxysilicane) in, concentration of the graphene oxide in silane coupling agent is 7.5g/L, then
N is added, N- dicyclohexylcarbodiimide, N, concentration of the N- dicyclohexylcarbodiimide in silane coupling agent is 7.5g/L, is surpassed
Sound disperses 60min (it is 150W that ultrasonic wave, which disperses power), obtains graphene oxide dispersion, is transferred in reactor at 70 DEG C anti-
Reaction mixture should be consolidated through filtration washing vacuum drying (vacuum drying temperature is 50 DEG C, drying time 48h) for 24 hours
Body powder, restored (restoring method be first with 1% liquor kalii iodide reduction treatment 4h, after with 2% hydrazine hydrate solution reduction treatment
Modified graphene oxide is obtained after 4h)；
Step (2) modified polyorganosiloxane preparation: by siloxanyl monomers (octamethylcy-clotetrasiloxane), silane coupling agent (3-
(2,3 the third oxygen of epoxy) propyl-triethoxysilicane, triethoxysilane), end-capping reagent (hexamethyldisiloxane), catalyst (hydrogen
Lithia), crosslinking agent (the third chlorine of epoxy) react 5h at 120 DEG C, obtain modified polyorganosiloxane；Wherein, the silane coupling agent
Concentration is 1%, and the end-capping reagent concentration is 0.4%, and the catalyst concn is 0.12%, and the crosslinker concentration is
0.4%；
The graphene-based polysiloxanes preparation of step (3) silicon oxygen six-membered ring structure: deionization is added in modified graphene oxide
In water, the concentration of modified graphene oxide in deionized water is 5g/L, and (ultrasonic wave disperses power to ultrasonic disperse 30min
150W), modified graphene oxide dispersion liquid is obtained；Modified polyorganosiloxane is added in modified graphene oxide dispersion liquid, it is modified
Concentration of the polysiloxanes in modified graphene oxide dispersion liquid is 750g/L, triethylamine is added, triethylamine is in modified oxidized stone
Concentration in black alkene dispersion liquid is 0.015g/L, and colloidal sol is made in 6h under 10 DEG C of reactions, is then warming up to 70 DEG C of reaction 3h and is made
Gel solution will obtain gel after gel solution vacuum drying (vacuum drying temperature is 50 DEG C, drying time 48h),
The graphene-based poly- silicon oxygen of silicon oxygen six-membered ring structure is obtained after being restored (restoring method is the reduction treatment 30min at 100 DEG C) again
Alkane.
The preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure in summary, effectively promotion graphene oxide
Dispersion stabilization in polysiloxanes, realizes the effective compound of graphene oxide and polysiloxanes, effectively by polysiloxanes and
Graphene has complementary advantages, and providing one kind has strong certain conductive capability, physical property height, mechanical strength, color inhibition, using the longevity
The water-soluble graphene modified polyorganosiloxane material of the excellent properties such as life length.
In order to which the technology of the graphene-based polysiloxanes preparation method of silicon oxygen six-membered ring structure described in further instruction is imitated
Fruit carries out the Experimental comparison of application examples 1 and Comparison study example 1-2, wherein application examples 1 and Comparison study example 1-2 compounding skin used
The method for removing from office upper layer finishing agent is consistent, and difference is only that: application examples 1 is that silicon oxygen obtained by the embodiment of the present invention 1 is hexa-atomic
The graphene-based silicone materials of ring structure are compounded with nitrocotton brightener is made leather upper layer finishing agent, and Comparison study example 1 is
It will be compounded without modified polysiloxanes with nitrocotton brightener and leather upper layer finishing agent be made, Comparison study example 2 is direct
Leather upper layer finishing agent only is made with nitrocotton brightener, specific amounts of components is as shown in table 1 below.To respectively use application examples
Coating obtained by the leather upper layer finishing agent of 1 and Comparison study example 1-2 carries out performance comparison, and comparing result is as shown in table 2 below.
1 leather upper layer finishing agent dosage of each component of table
2 leather upper layer finishing agent coating testing result of table
Shown in sum up, the graphene-based polysiloxanes of silicon oxygen six-membered ring structure made from preparation method is answered through the invention
When for leather upper layer finishing agent, wear-resisting, resistance to dry/wet rubbing of gained leather coating, static water absorption performance are obviously improved.Cause
This, the present invention uses graphene oxide for graphene raw material, is modified using sol-gal process to polysiloxanes, reacts item
Part is mild, it is modified restore after graphene defect it is few, to improve the graphene-based polysiloxanes of silicon oxygen six-membered ring structure
Service life, the silicon oxygen six-membered ring structure of preparation graphene-based silicone materials purity is high meets industrialized production and essence
The requirement of thin chemical industry, improves the physical property and mechanical strength of polysiloxanes, promotes it using practicability.
The foregoing descriptions are merely the embodiment using this origination techniques content, any those skilled in the art use this wound
Make done modifications and changes, all belong to the scope of the patents of this creation opinion, and is not limited to those disclosed embodiments.
Claims (10)
1. a kind of preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure, which comprises the steps of:
Step (1) graphene oxide is modified: adding graphene oxide into silane coupling agent, N, N- dicyclohexyl is then added
Carbodiimide, ultrasonic disperse 20-200min, obtains graphene oxide dispersion, is transferred in reactor and reacts at 50-100 DEG C
Reaction mixture is dried in vacuo to obtain solid powder through filtration washing, obtains modified graphene oxide after carrying out reduction by 12-72h；
Step (2) modified polyorganosiloxane preparation: by siloxanyl monomers, silane coupling agent, end-capping reagent, catalyst, crosslinking agent in 70-
3-8h is reacted at 140 DEG C, obtains modified polyorganosiloxane；
The graphene-based polysiloxanes preparation of step (3) silicon oxygen six-membered ring structure: modified graphene oxide is added in deionized water,
Ultrasonic disperse 20-200min, obtains modified graphene oxide dispersion liquid；Modified graphene oxide point is added in modified polyorganosiloxane
In dispersion liquid, triethylamine is added, colloidal sol is made in 3-8h under 10-50 DEG C of reaction, is then warming up to 60-100 DEG C of reaction 1-5h system
Obtain gel solution；Gel is obtained after gel solution is dried in vacuo, then obtains silicon oxygen six-membered ring structure graphite after carrying out reduction
Alkenyl silicone materials.
2. the preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure according to claim 1, it is characterised in that:
Silane coupling agent described in step (1) is at least 3- chloropropyl triethoxysilane, 3- aminopropyl triethoxysilane, 3- (2,3
The third oxygen of epoxy) propyl-triethoxysilicane, one of triethoxysilane.
3. the preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure according to claim 1, it is characterised in that:
Concentration of the graphene oxide in silane coupling agent described in step (1) is 1-15g/L, and the catalyst is in silane coupling agent
Concentration be 1-15g/L.
4. the preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure according to claim 1, it is characterised in that:
Siloxanyl monomers described in step (2) are octamethylcy-clotetrasiloxane.
5. the preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure according to claim 1, it is characterised in that:
Silane coupling agent described in step (2) is at least 3- chloropropyl triethoxysilane, 3- aminopropyl triethoxysilane, 3- (2,3
The third oxygen of epoxy) propyl-triethoxysilicane, one of triethoxysilane.
6. the preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure according to claim 1, it is characterised in that:
End-capping reagent described in step (2) be at least 1,3- bis- (3- glycydoxy) -1,1,3,3- tetramethyl disiloxane,
One of hexamethyldisiloxane.
7. the preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure according to claim 1, it is characterised in that:
Catalyst described in step (2) is at least one of potassium hydroxide, lithium hydroxide, tetramethylammonium hydroxide.
8. the preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure according to claim 1, it is characterised in that:
Crosslinking agent described in step (2) is at least one of epoxy prapanol, third chlorine of epoxy.
9. the preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure according to claim 1, it is characterised in that:
The concentration of silane coupling agent described in step (2) is 0.1-5%, and the end-capping reagent concentration is 0.1-1%, and the catalyst is dense
Degree is 0.01-0.2%, and the crosslinker concentration is 0-4%.
10. the preparation method of the graphene-based polysiloxanes of silicon oxygen six-membered ring structure according to claim 1, feature exist
In: the concentration of modified graphene oxide in deionized water described in step (3) is 0.5-10g/L；The modified polyorganosiloxane
Concentration in modified graphene oxide dispersion liquid is 100-1000g/L, and the triethylamine disperses in modified graphene oxide
Concentration in liquid is 0.005-0.025g/L.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110330652A (en) * | 2019-06-26 | 2019-10-15 | 兴业皮革科技股份有限公司 | A kind of preparation method of the graphene-based polysiloxanes of low-viscosity and the method for reducing graphene-based silicone cross degree |
| CN110628960A (en) * | 2019-09-09 | 2019-12-31 | 兴业皮革科技股份有限公司 | Production process of thick natural pattern-falling high-grade sofa leather |
| CN114657707A (en) * | 2022-05-19 | 2022-06-24 | 南通大学 | Preparation method of waterproof, moisture-permeable and antibacterial nanofiber membrane |
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| CN110628960A (en) * | 2019-09-09 | 2019-12-31 | 兴业皮革科技股份有限公司 | Production process of thick natural pattern-falling high-grade sofa leather |
| CN110628960B (en) * | 2019-09-09 | 2021-06-15 | 兴业皮革科技股份有限公司 | Production process of thick natural pattern-falling high-grade sofa leather |
| CN114657707A (en) * | 2022-05-19 | 2022-06-24 | 南通大学 | Preparation method of waterproof, moisture-permeable and antibacterial nanofiber membrane |
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