CN106750335A - A kind of organosilicon Graphene complex microsphere - Google Patents
A kind of organosilicon Graphene complex microsphere Download PDFInfo
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- CN106750335A CN106750335A CN201611120211.4A CN201611120211A CN106750335A CN 106750335 A CN106750335 A CN 106750335A CN 201611120211 A CN201611120211 A CN 201611120211A CN 106750335 A CN106750335 A CN 106750335A
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- organosilicon
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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
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
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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
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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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
- C08J2383/10—Block- or graft-copolymers containing polysiloxane sequences
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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
- C08J2387/00—Characterised by the use of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
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Abstract
A kind of organosilicon Graphene complex microsphere, belongs to organosilicon and technical field of emulsion polymerization.The present invention forms emulsion by mixture of the Graphene stable emulsifying containing vinyl silicone oil (or the linear diolefin of α, ω) and containing hydrogen silicone oil, then prepares organosilicon Graphene complex microsphere by Si―H addition reaction crosslinking.The organosilicon Graphene complex microsphere anti-agglomeration is strong, be easily dispersed, and with the intensity of the elasticity, flexibility and Graphene of organosilicon, can be used for the activeness and quietness of plastics, coating and rubber, it can also be used to play the screening flaw, smooth in cosmetics.
Description
Technical field
The present invention relates to organosilicon Graphene complex microsphere, the more particularly to organic silicon emulsion of Graphene stable emulsifying gathers
Close.Belong to organosilicon and technical field of emulsion polymerization.
Background technology
Organosilicone elastic microballoon is due to being mainly used as the modified of synthetic resin with excellent flexibility, super-hydrophobicity
Agent, the surface modifier of coating, cosmetics and fiber, the additive of leather treatment etc..Organosilicone elastic microballoon is used for thermoplastic
Property and thermosetting resin to improve their shock resistance, for increasing its lubricity in coating.However, due to organosilicon
Flexibility and make the intensity decreases of material.The organosilicon Graphene that the present invention is prepared by the method for Pickering emulsion polymerizations
Complex microsphere, the high intensity of flexibility and Graphene with organosilicon can be widely applied to plastics, rubber and coating neck
Domain.
The content of the invention
It is an object of the invention to provide a kind of organosilicon Graphene complex microsphere and preparation method thereof.
A kind of organosilicon Graphene complex microsphere of the invention, its volume average size is 0.5~200 μm, and Graphene contains
It is 1%-20% to measure, and silicone content is 80-99%.
Specifically preparation process is：
(1) compound and containing hydrogen silicone oil containing two or more double bonds are mixed, its mixed proportion is rubbed for Shuan Jian ︰ hydrogen
You are than being 0.1-2:1；
(2) by the material prepared in step (1), the Graphene of the 1wt%-25wt% for accounting for the material prepared in step (1),
With Pt account for the quality of material prepared in step (1) be calculated as the platinum catalyst of 1-100ppm and with the material for preparing in step (1)
Weight is than the water mixing for 0.65-10 times and homogeneous forms emulsion, and Si―H addition reaction crosslinking is carried out at room temperature, if cannot react completely
Entirely, can be heated to be carried out at less than 100 DEG C, reaction is ground after emulsion is vacuum dried or is spray-dried after terminating and obtained final product
Machine 3 SiC 2/graphite alkene complex microsphere.
The compound containing two or more double bonds is dimethyl silicone polymer or α, ω containing vinyl-linear
Diolefin；
Dimethyl silicone polymer containing vinyl, its structural formula is：
ViSiMe2O(SiMe2O)pSiMe2V；Or Me3SiO(SiMe2O)m(SiMeVi)nSiMe3
Wherein Me and Vi are respectively methyl and vinyl, and p, m, n is respectively 10-600, the integer of 10-1000,2-50；
The molecular formula of the α, ω-linear diolefin is CH2CH(CH2)aCHCH2, a is the integer of 1-20.
The containing hydrogen silicone oil activity hydrogen mole fraction content is 0.06%-6.0%, and its structural formula is：
Me3SiO(Me2SiO)q(MeHSiO)rSiMe3
Wherein Me is methyl, and q, r is respectively 0-200, the integer of 8-100.
Described platinum catalyst is selected from：Chloroplatinic acid；Chloroplatinate；The modified chloroplatinic acid of alcohol；The cooperation of chloroplatinic acid and alkene
Thing；The complex of chloroplatinic acid, chloroplatinate and the siloxanes containing vinyl.
Brief description of the drawings
The microphotograph of the organosilicon Graphene complex microsphere of Fig. 1 embodiments 1.
Specific embodiment
The invention will be further elaborated for the following examples, it is therefore intended that be best understood from present disclosure rather than
Limit the scope of the invention.
Embodiment 1：
(1) by 10g viscosity 200cSt vinyl-terminated silicone oil (double bond contents 2.5 × 10-4) and 0.5g viscosity mol/g
100cSt containing hydrogen silicone oils (hydrogen content 5 × 10-3Mol/g) (vinyl and hydrogen mol ratio are 1 for mixing:1).Add 5.575 × 10-5g
Chloroplatinic acid (accounting for mixture gauge 2ppm by Pt).
(2) 0.12g Graphenes addition 12g water is stirred.
(3) (1) described mixture and (2) described mixture are mixed and homogeneous formation emulsion, 24h is reacted at 20 DEG C.Will
Emulsion grinds to obtain organosilicon Graphene complex microsphere after drying.
Organosilicon Graphene complex microsphere microphotograph is by VHX-1000 digit microscopes (Keyence
Int.Trading Co.Ltd., Japan) shoot.Fig. 1 is the microphotograph of organosilicon Graphene complex microsphere.It can be seen that
Ball-type microballoon is formd, at 28-170 μm, microsphere surface is Graphene to size.
Embodiment 2：
(1) by 10g viscosity 20cSt vinyl silicone oil (contents of ethylene 1.1 × 10-3) and 1.375g viscosity mol/g
100cSt containing hydrogen silicone oils (hydrogen content 1.6 × 10-2Mol/g) (vinyl and hydrogen mol ratio are 1 for mixing:2) 1.51, are added ×
10-4The chloroplatinic acid (accounting for mixture gauge 5ppm by Pt) of g.
(2) aqueous dispersions are configured in 2.8g Graphenes being added into 100g water.
(3) (1) described mixture and (2) described aqueous dispersions are mixed and homogeneous formation emulsion, 12h is reacted at 50 DEG C.
Organosilicon Graphene complex microsphere is ground to obtain after emulsion is dried.
Unless spirit of the invention is not substantially met, the word " bag used when material or raw material is enumerated in the application
Include ", any mixture or composition including specified raw material such as " being selected from ".
All bibliography, patent, patent application, public publication for being referred in this specification etc., by quoting simultaneously
In entering the application.
In this application, unless expressly stated otherwise, when number range is referred to, including scope end points；Specified
Each value and its subrange in number range are regarded as specifically writing out, and are included in the application particularly disclosed scope
It is interior.
It should be understood that after the application is read, those skilled in the art will can be readily derived the embodiment of the present application
Various modifications and remodeling.Therefore, the invention is not restricted to shown embodiment, and should include within all spirit and scope of the invention
All modifications and remodeling.
Claims (5)
1. a kind of organosilicon Graphene complex microsphere, it is characterised in that the microsphere volume average-size is 0.5~200 μm, graphite
Alkene content is 1%-20%, and silicone content is 80-99%.
2. the organosilicon Graphene complex microsphere of the requirement of right 1 contains two or more double bonds by Graphene stable emulsifying
Compound and containing hydrogen silicone oil form emulsion, are then crosslinked by Si―H addition reaction and formed, and specific preparation process is：
(1) compound and containing hydrogen silicone oil containing two or more double bonds are mixed, its mixed proportion is Shuan Jian ︰ hydrogen mol ratios
It is 0.1-2:1；
(2) by the material prepared in step (1), the Graphene of the 1wt%-25wt% for accounting for the material prepared in step (1), with Pt
Account for the quality of material prepared in step (1) and be calculated as the platinum catalyst of 1-100ppm and the weight with the material of preparation in step (1)
Than the water mixing for 0.65-10 times and homogeneous formation emulsion, Si―H addition reaction crosslinking is carried out at room temperature, if reaction is incomplete,
Can be heated to less than carrying out at 100 DEG C, reaction emulsion is vacuum dried or is spray-dried after terminating after grinding obtain final product it is organic
3 SiC 2/graphite alkene complex microsphere.
3. the preparation method of organosilicon Graphene complex microsphere according to claim 2, it is characterised in that it is described contain two or
The compound of two or more double bond is dimethyl silicone polymer or α, ω containing vinyl-linear diolefin；
Dimethyl silicone polymer containing vinyl, its structural formula is：
ViSiMe2O(SiMe2O)pSiMe2V；Or Me3SiO(SiMe2O)m(SiMeVi)nSiMe3
Wherein Me and Vi are respectively methyl and vinyl, and p, m, n is respectively 10-600, the integer of 10-1000,2-50；
The molecular formula of the α, ω-linear diolefin is CH2CH(CH2)aCHCH2, a is the integer of 1-20.
4. the preparation method of organosilicon Graphene complex microsphere according to claim 2, it is characterised in that the Silicon Containing Hydrogen
Oily activity hydrogen mole fraction content is 0.06%-6.0%, and its structural formula is：
Me3SiO(Me2SiO)q(MeHSiO)rSiMe3
Wherein Me is methyl, and q, r is respectively 0-200, the integer of 8-100.
5. the preparation method of organosilicon Graphene complex microsphere according to claim 2, it is characterised in that described platinum is urged
Agent is selected from：Chloroplatinic acid；Chloroplatinate；The modified chloroplatinic acid of alcohol；The complex of chloroplatinic acid and alkene；Chloroplatinic acid, chloroplatinate
With the complex of the siloxanes containing vinyl.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109651816A (en) * | 2018-11-20 | 2019-04-19 | 兴业皮革科技股份有限公司 | A kind of compound emulsion method of graphene-based polysiloxanes |
| CN110093040A (en) * | 2019-06-05 | 2019-08-06 | 华东交通大学 | Additive and preparation method, PP/PET blending modified material and preparation method |
| WO2021028702A1 (en) * | 2019-08-14 | 2021-02-18 | The University Of Sussex | Composite materials made from Pickering emulsions |
| CN116463785A (en) * | 2023-02-22 | 2023-07-21 | 芯安健康科技(广东)有限公司 | Multifunctional healthy fiber sheet and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421191A (en) * | 2013-08-14 | 2013-12-04 | 江南大学 | Organic silicon elastic microsphere preparation method |
-
2016
- 2016-12-08 CN CN201611120211.4A patent/CN106750335A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421191A (en) * | 2013-08-14 | 2013-12-04 | 江南大学 | Organic silicon elastic microsphere preparation method |
Non-Patent Citations (1)
| Title |
|---|
| KIM SD: "Pickering emulsion-fabricated polystyrene–graphene oxide microspheres and their electrorheology", 《JOURNAL OF MATERIALS CHEMISTRY C》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109651816A (en) * | 2018-11-20 | 2019-04-19 | 兴业皮革科技股份有限公司 | A kind of compound emulsion method of graphene-based polysiloxanes |
| CN109651816B (en) * | 2018-11-20 | 2021-06-15 | 兴业皮革科技股份有限公司 | Compound emulsification method of graphene-based polysiloxane |
| CN110093040A (en) * | 2019-06-05 | 2019-08-06 | 华东交通大学 | Additive and preparation method, PP/PET blending modified material and preparation method |
| WO2021028702A1 (en) * | 2019-08-14 | 2021-02-18 | The University Of Sussex | Composite materials made from Pickering emulsions |
| CN116463785A (en) * | 2023-02-22 | 2023-07-21 | 芯安健康科技(广东)有限公司 | Multifunctional healthy fiber sheet and preparation method and application thereof |
| CN116463785B (en) * | 2023-02-22 | 2024-01-23 | 芯安健康科技(广东)有限公司 | Multifunctional healthy fiber sheet and preparation method and application thereof |
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