CN106432786A - Method for preparing efficiently hydrophobic and oil-absorbing sponge with fluorine-containing silane coupling agent as cross-linking agent - Google Patents
Method for preparing efficiently hydrophobic and oil-absorbing sponge with fluorine-containing silane coupling agent as cross-linking agent Download PDFInfo
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- CN106432786A CN106432786A CN201610845619.1A CN201610845619A CN106432786A CN 106432786 A CN106432786 A CN 106432786A CN 201610845619 A CN201610845619 A CN 201610845619A CN 106432786 A CN106432786 A CN 106432786A
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- oil
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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
- C08J9/36—After-treatment
- C08J9/40—Impregnation
- C08J9/42—Impregnation with macromolecular compounds
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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
- C08J9/36—After-treatment
- C08J9/40—Impregnation
- C08J9/405—Impregnation with polymerisable compounds
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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
- C08J2483/00—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
- C08J2483/04—Polysiloxanes
- C08J2483/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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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
- C08J2483/00—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
- C08J2483/04—Polysiloxanes
- C08J2483/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
Abstract
The invention discloses a method for preparing an efficiently hydrophobic and oil-absorbing sponge with a fluorine-containing silane coupling agent as a cross-linking agent. According to the method, a porous sponge is taken as a base body, an organosilicone hydrophobic layer is formed on the surface of the sponge through simple soaking and curing operations, the original water-absorbing and oil-absorbing amphiphilic sponge becomes a hydrophobic and oil-absorbing selective sponge, and the method is a surface modification method with which the performance of the sponge can be changed simply and efficiently. The original high porosity of the porous sponge is remained due to the organosilicone hydrophobic layer, and efficiently hydrophobic and oil absorbing characteristics are obtained. According to the method, the preparation process is simple, the reaction conditions are mild, raw materials are low in price and easy to obtain, and the prepared sponge has oil-water selective absorption, enables oil and water to be quickly, efficiently and automatically separated, has high oil storage capacity and recycling performance and can be squeezed repeatedly for recovery of oils.
Description
Technical field
The invention belongs to functional high molecule material and material surface modify field, relate to one kind succinctly efficiently hydrophobic oil suction
Sponge preparation and in particular to a kind of with fluorine containing silane coupling agent for cross-linking agent prepare efficiently hydrophobic oil suction sponge method.
Background technology
Ocean oil spill accident, industrial wastewater discharge and organic solvent leakage cause permanent to ecological environment and system
Infringement, traditional oily water separation technique is such as：Combustion in situ method, Filtration, gravitational separation process and chemical reagent add method etc. because of it
High cost and produce little effect and be restricted, researchs and develops efficient water-oil separating material extremely urgent.Surface and interface for material
Making rapid progress of technology brings opportunity to develop for oily water separation technique, and super-hydrophobic oleophylic sponge is then effective cleaning oil pollution
One of material.Sponge has high opening rate and big specific surface area in itself, can store a large amount of oil products, it is amphipathic limit wide
General application.By surface simply modify change its amphipathic possess selection absorbability, become high efficiency oil-water separation material.This three
, because having high porosity, bigger serface and high oil storage capacity, need not collect polluted source can for the three-dimensional water-oil separating material of dimension
Realize efficiently and rapidly profit to be automatically separated.Therefore, 3 D stereo water-oil separating material be rapidly and efficiently process crude oil leakage and
The optimum selection of oil pollution, is conducive to tackling various burst marine oil spills and oil leak event.The present invention is by sponge
Simple immersion solidification makes it possess organic silicon hydrophobic layer and possess selection absorbability, the efficiently hydrophobic oil suction of prepared 3 D stereo
Succinctly quick, oil absorbency is high and reuse capable of circulation for sponge preparation process, has broken the constraint of traditional material and method, be containing
Oily sewage disposal, industrial oil pollutant separate and ocean oil spill accident provides cheap and efficiently quick processing scheme.
Content of the invention
It is an object of the invention to improving existing water-oil separating material preparation process complexity, high cost, low the lacking of oil absorbency
Fall into, a kind of method preparing efficiently hydrophobic oil suction sponge for cross-linking agent with fluorine containing silane coupling agent is provided.
Concretely comprise the following steps：
(1) organic silicon emulsion immersion is obtained with cross-linking agent after aqueous emulsion of dimethyl polysiloxane fluid being mixed homogeneously.
(2) mandruka being dried after washing is immersed in the organic silicon emulsion immersion that step (1) is obtained, ultrasonic disperse soaks
Bubble uniformly takes out mandruka afterwards and removes immersion more than needed, is subsequently placed in dry solidification in 20 ~ 150 DEG C of vacuum drying oven extremely permanent
Weight, that is, be obtained efficiently hydrophobic oil suction sponge.
Described aqueous emulsion of dimethyl polysiloxane fluid is hydroxy-end capped aqueous emulsion of dimethyl polysiloxane fluid, and its solid content is 5 ~ 50%.
Described cross-linking agent is fluorine containing silane coupling agent, preferably trifluoro propyl trichlorosilane, trifluoro propyl triethoxysilane
Or PFPE siloxanes, and consumption is 0.5 ~ 8 wt% of polydimethylsiloxane.
The present invention has advantages below：
(1) preparation process is simple of the inventive method, reaction condition is gentle, and raw material is cheap and easy to get.
(2) sponge of present invention preparation has profit selection absorbability, is capable of profit and is rapidly and efficiently automatically separated.
(3) sponge of present invention preparation has high oil storage capacity and recycling ability, can repeatedly extrude oil recovery
Product.
Brief description
Fig. 1 is the scanning electron microscopy of the efficiently hydrophobic oil suction sponge that untreated sponge and the embodiment of the present invention 1 are obtained
Mirror photo（A is the SEM photograph of untreated sponge；B is the SEM photograph of efficiently hydrophobic oil suction sponge）.
Fig. 2 is the lyophobic oil-absorption pair of the efficiently hydrophobic oil suction sponge that untreated sponge and the embodiment of the present invention 1 are obtained
According to piece.
Fig. 3 is oil suction state photo in oil-water mixture for the prepared efficiently hydrophobic oil suction sponge of the embodiment of the present invention 1.
Specific embodiment
Embodiment 1：
Aqueous isopropanol by 3 mL silane coupler PFPE siloxanes（Mass content 10%）It is added dropwise to 50 g hydroxyls
The aqueous emulsion of dimethyl polysiloxane fluid of base end-blocking（Solid content 30%）In, organic silicon emulsion immersion is obtained after being uniformly mixed；By water
The mandruka being dried after washing is immersed in immersion, ultrasonic disperse 5 min, soaks and uniformly takes out mandruka afterwards and extrude more than needed
Immersion, solidifies 8 h to constant weight, that is, efficiently hydrophobic oil suction sponge is obtained in the vacuum drying oven being subsequently placed in 90 DEG C.
Embodiment 2：
Aqueous isopropanol by 3 mL silane coupler PFPE siloxanes（Mass content 10%）It is added dropwise to 50 g hydroxyls
The aqueous emulsion of dimethyl polysiloxane fluid of base end-blocking（Solid content 30%）In, organic silicon emulsion immersion is obtained after being uniformly mixed；By water
The mandruka being dried after washing is immersed in immersion, ultrasonic disperse 5 min, soaks and uniformly takes out mandruka afterwards and extrude more than needed
Immersion, is subsequently placed in solidification 10h in 80 DEG C of vacuum drying oven and to constant weight, that is, efficiently hydrophobic oil suction sponge is obtained.
Embodiment 3：
Aqueous isopropanol by 3 mL silane coupler PFPE siloxanes（Mass content 10%）It is added dropwise to 75 g hydroxyls
The aqueous emulsion of dimethyl polysiloxane fluid of base end-blocking（Solid content 20%）In, organic silicon emulsion immersion is obtained after being uniformly mixed；By water
The mandruka being dried after washing is immersed in immersion, ultrasonic disperse 5 min, soaks and uniformly takes out mandruka afterwards and extrude more than needed
Immersion, is subsequently placed in solidification 10h in 80 DEG C of vacuum drying oven and to constant weight, that is, efficiently hydrophobic oil suction sponge is obtained.
Embodiment 4：
Aqueous isopropanol by 4 mL silane coupler PFPE siloxanes（Mass content 10%）It is added dropwise to 50 g hydroxyls
The aqueous emulsion of dimethyl polysiloxane fluid of base end-blocking（Solid content 30%）In, organic silicon emulsion immersion is obtained after being uniformly mixed；By water
The mandruka being dried after washing is immersed in immersion, ultrasonic disperse 5 min, soaks and uniformly takes out mandruka afterwards and extrude more than needed
Immersion, solidifies 8 h to constant weight, that is, efficiently hydrophobic oil suction sponge is obtained in the vacuum drying oven being subsequently placed in 90 DEG C.
Embodiment 5：
Aqueous isopropanol by 2 mL silane coupler PFPE siloxanes（Mass content 10%）It is added dropwise to 50 g hydroxyls
The aqueous emulsion of dimethyl polysiloxane fluid of base end-blocking（Solid content 30%）In, organic silicon emulsion immersion is obtained after being uniformly mixed；By water
The mandruka being dried after washing is immersed in immersion, ultrasonic disperse 5 min, soaks and uniformly takes out mandruka afterwards and extrude more than needed
Immersion, solidifies 8 h to constant weight, that is, efficiently hydrophobic oil suction sponge is obtained in the vacuum drying oven being subsequently placed in 90 DEG C.
Embodiment 6：
500 μ L silane coupler trifluoro propyl triethoxysilanes are added dropwise to the hydroxy-end capped poly dimethyl silicon of 90 g
Oxygen alkane emulsion（Solid content 30%）In, organic silicon emulsion immersion is obtained after being uniformly mixed；The mandruka being dried after washing
It is immersed in immersion, ultrasonic disperse 5 min, soak and uniformly take out mandruka afterwards and extrude immersion more than needed, be subsequently placed in 90 DEG C
Vacuum drying oven in solidify 8 h to constant weight, that is, efficiently hydrophobic oil suction sponge is obtained.
Embodiment 7：
500 μ L silane coupler trifluoro propyl trichlorosilanes are added dropwise to the hydroxy-end capped polydimethylsiloxane of 90 g
Emulsion（Solid content 30%）In, organic silicon emulsion immersion is obtained after being uniformly mixed；The mandruka being dried after washing is soaked
In immersion, ultrasonic disperse 5 min, soaks and uniformly takes out mandruka extrude immersion more than needed afterwards, be subsequently placed in 90 DEG C true
Solidify 8 h in empty drying baker to constant weight, that is, efficiently hydrophobic oil suction sponge is obtained.
Claims (2)
1. a kind of method with fluorine containing silane coupling agent for the cross-linking agent efficiently hydrophobic oil suction sponge of preparation is it is characterised in that concrete walk
Suddenly it is：
(1) organic silicon emulsion immersion is obtained with cross-linking agent after aqueous emulsion of dimethyl polysiloxane fluid being mixed homogeneously；
(2) mandruka being dried after washing is immersed in the organic silicon emulsion immersion that step (1) is obtained, ultrasonic disperse soaks all
Take out mandruka after even and remove immersion more than needed, be subsequently placed in 20 ~ 150 DEG C of vacuum drying oven dry solidification to constant weight, that is,
Efficiently hydrophobic oil suction sponge is obtained；
Described aqueous emulsion of dimethyl polysiloxane fluid is hydroxy-end capped aqueous emulsion of dimethyl polysiloxane fluid, and its solid content is 5 ~ 50%；
Described cross-linking agent is fluorine containing silane coupling agent, and its consumption is 0.5 ~ 8 wt% of polydimethylsiloxane.
2. the method that efficiently hydrophobic oil suction sponge is prepared for cross-linking agent with fluorine containing silane coupling agent according to claim 1,
It is characterized in that described fluorine containing silane coupling agent is trifluoro propyl trichlorosilane, trifluoro propyl triethoxysilane or PFPE
Siloxanes.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610845619.1A CN106432786A (en) | 2016-09-26 | 2016-09-26 | Method for preparing efficiently hydrophobic and oil-absorbing sponge with fluorine-containing silane coupling agent as cross-linking agent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610845619.1A CN106432786A (en) | 2016-09-26 | 2016-09-26 | Method for preparing efficiently hydrophobic and oil-absorbing sponge with fluorine-containing silane coupling agent as cross-linking agent |
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| CN106432786A true CN106432786A (en) | 2017-02-22 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109181005A (en) * | 2018-07-11 | 2019-01-11 | 赵建平 | The preparation method of greasy dirt Wiping material is received in a kind of high friction |
| CN109400946A (en) * | 2018-11-02 | 2019-03-01 | 郑州峰泰纳米材料有限公司 | A kind of preparation method that hydrophobicity melamine bubble is continuous |
| CN110777539A (en) * | 2019-11-18 | 2020-02-11 | 塔里木大学 | Preparation method of water-repellent oil-absorbing three-dimensional porous cotton fabric |
| CN113813937A (en) * | 2021-11-03 | 2021-12-21 | 江苏大学 | Selective adsorption material and preparation method thereof |
| CN115069227A (en) * | 2022-06-17 | 2022-09-20 | 浙江工业大学 | Hydrophobic oil absorption sponge for oil-water separation and preparation method thereof |
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| CN102660046A (en) * | 2012-05-11 | 2012-09-12 | 北京航空航天大学 | Preparation method of superhydrophobic/superoleophilic sponge |
| CN105797431A (en) * | 2016-03-28 | 2016-07-27 | 桂林理工大学 | Method for preparing efficient hydrophobic oil-absorbing sponge |
| CN105949498A (en) * | 2016-05-19 | 2016-09-21 | 北京林业大学 | Melamine-based sponge for absorbing oil slick and preparation method |
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2016
- 2016-09-26 CN CN201610845619.1A patent/CN106432786A/en active Pending
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| CN102660046A (en) * | 2012-05-11 | 2012-09-12 | 北京航空航天大学 | Preparation method of superhydrophobic/superoleophilic sponge |
| CN105797431A (en) * | 2016-03-28 | 2016-07-27 | 桂林理工大学 | Method for preparing efficient hydrophobic oil-absorbing sponge |
| CN105949498A (en) * | 2016-05-19 | 2016-09-21 | 北京林业大学 | Melamine-based sponge for absorbing oil slick and preparation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109181005A (en) * | 2018-07-11 | 2019-01-11 | 赵建平 | The preparation method of greasy dirt Wiping material is received in a kind of high friction |
| CN109400946A (en) * | 2018-11-02 | 2019-03-01 | 郑州峰泰纳米材料有限公司 | A kind of preparation method that hydrophobicity melamine bubble is continuous |
| CN110777539A (en) * | 2019-11-18 | 2020-02-11 | 塔里木大学 | Preparation method of water-repellent oil-absorbing three-dimensional porous cotton fabric |
| CN113813937A (en) * | 2021-11-03 | 2021-12-21 | 江苏大学 | Selective adsorption material and preparation method thereof |
| CN115069227A (en) * | 2022-06-17 | 2022-09-20 | 浙江工业大学 | Hydrophobic oil absorption sponge for oil-water separation and preparation method thereof |
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Application publication date: 20170222 |
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