CN105080185B - Interpenetrating network type porous polymer with adjustable and controllable surface performance and preparation method of interpenetrating network type porous polymer - Google Patents
Interpenetrating network type porous polymer with adjustable and controllable surface performance and preparation method of interpenetrating network type porous polymer Download PDFInfo
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- CN105080185B CN105080185B CN201510502804.6A CN201510502804A CN105080185B CN 105080185 B CN105080185 B CN 105080185B CN 201510502804 A CN201510502804 A CN 201510502804A CN 105080185 B CN105080185 B CN 105080185B
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Abstract
The invention discloses an interpenetrating network type porous polymer with adjustable and controllable surface performance and a preparation method of the interpenetrating network type porous polymer. The interpenetrating network type porous polymer is characterized by comprising a main body made from a porous material, wherein a layer of silicone rubber/paraffin microsphere compounds consisting of silicone rubber and paraffin microspheres is polymerized on a three-dimensional porous structure of the main body. According to the interpenetrating network type porous polymer with the adjustable and controllable surface performance and the preparation method of the interpenetrating network type porous polymer, continuous separation and recovery of an oil phase are achieved, the separation efficiency of oil contamination and the efficiency of environmental restoration can be significantly improved, the preparation cost is low, the process is simple, and a preparation process is green and pollution-free and has broad application prospect in the field of oil-water two-phase separation.
Description
Technical field
The present invention relates to regulatable porous polymer of a kind of intercrossed network type surface property and preparation method thereof, especially relates to
And it is a kind of for regulatable porous polymer of the detached intercrossed network type surface property of oil/water and preparation method thereof, belonging to has
Machine solvent and water two-phase laminated flow technical field.
Background technology
If oily waste water is not recycled, can cause to waste；Oily waste water enters river, lake or bay, meeting
Polluted-water, affects aquatile existence；Oily waste water is used for agricultural irrigation, then can block interstices of soil, hinders crops life
It is long.Oily waste water is discharged to after the water bodys such as rivers,lakes and seas, and oil reservoir covers the water surface, prevents the oxygen in air to the diffusion in water.Water
Because dissolved oxygen is reduced in body, the photosynthesis that algae is carried out is restricted；Hydrobiological normal growth is affected, is made aquatic dynamic
Plant has oily taste or toxicity, or even makes water body foul, and destroys the value of water resource.If livestock has drunk oily waste water, lead to
Fatal esophageal disease can often be infected.If using oily waste water irrigated farmland, oil and its derivative are by mulching soil and plant
Surface, blocks the hole of soil, prevents air from penetrating, and makes fruit have an oily taste, or prevent soil from be normally carried out metabolism and
Bacteria metabolism, can cause crop production reduction or death when serious.Further, since the drift and diffusion of oil spilling, can fall into disuse
Seabeach and seaside touring areas, cause great environmental hazard and social danger.But main harm is containing carcinogenic in oil
Hydrocarbon, is enriched with and is detrimental to health by food chain by fish, shellfish.
Oil spilling remedial technology the most frequently used at present includes oil skimmer, solidification Fei Ersi, dispersant, combustion biological prosthetic and in situ
Burn.These technologies only concentrate a large amount of oil dirt from water surface of cleaning, ignore adverse effect of the greasy dirt to environment in scattered water.Also go out at present
Show some oil leak repair materials, but most of oil leak repair materials are confined to volume and adsorbance material, also become obstruction
One big problem of current oil leak repair materials practical application.
The content of the invention
The technical problem to be solved is to provide a kind of specific surface area greatly, and pore structure is flourishing, constitutes continuous phase
Three-dimensional porous structure even, if continuous connected three-dimensional porous structure composition dry passage, the channel selectivity is strong, only allows oil phase
Pass through, realize continuous, the efficient separation to oil phase substance in oil water mixture, and be no longer limited to sorbing material from body
Product and adsorbance, can continuously use, without the need for the regulatable porous polymer of intercrossed network type surface property for regenerating；Further
Ground, the present invention provides a kind of intercrossed network type surface property regulatable poromeric preparation method, the method preparation cost
It is cheap, process is simple, preparation process green non-pollution, using silicon rubber and the hydrophobicity and lipophile of paraffin microballoon, with porous
Material is carrier, and as modifying agent, preparing can carry out the detached material of continuous water-oil phase to the paraffin microballoon with independent research；
Further, the present invention provides a kind of preparation method of the paraffin microballoon of micro-meter scale, and paraffin microballoon prepared by the method increases
Poromeric hydrophobicity of the present invention, increases selectivity of the passage to oil phase substance, and oil-water separation effect is good.
To solve above-mentioned technical problem, the technical solution used in the present invention is：
The regulatable porous polymer of intercrossed network type surface property, it is characterised in that：Including：Material is porous material
Main body, silicon rubber/paraffin microballoon that be polymerized in the three-dimensional cavernous structure of the main body one layer of silicon rubber and paraffin microballoon are constituted is answered
Compound.
The porous material includes polyurethane sponge.
The material of the silicon rubber includes 107-2000 double component room temperature vulcanization silicon rubbers.
The paraffin microballoon is the paraffin microballoon of micro-meter scale.
The regulatable poromeric preparation method of intercrossed network type surface property, it is characterised in that：Including following step
Suddenly：
S01, by main body of the material for porous material suitable size is cut into according to actual needs, is then placed in baking oven,
110~120oC is dried 1 ~ 2 hour；
S02, weighs in mass ratio silicon rubber and paraffin microballoon, and curing agent is added after stirring, then fully stirs
1 ~ 2min is mixed, mixed liquor is obtained；The mass ratio is silicon rubber：Paraffin microballoon=10 ~ 5:1；
S03, the main body in baking oven is taken out, and is put in the mixed liquor in step S02 and is fully absorbed, and is put after saturation to be absorbed
In entering baking oven, isothermal curing at least 2h obtains finished product.
Curing agent is producer's auxiliary products, generally the 1/10 of silicon rubber addition.
The preparation method of the paraffin microballoon is comprised the following steps：
Step one, adds water and surfactant in three-neck flask, places in 70 ~ 80 DEG C of thermostat water baths and heats 10
~ 15min, with electric mixer 2 ~ 3min is stirred；The addition of the surfactant is the 3 ~ 5 of the paraffin microspheres quality
Times；
Step 2, by the paraffin wax of solid-state, plus heat fusing, form liquid paraffin；With the speed of per minute 3 ~ 5 drops, delay
Slowly it is added drop-wise in the three-neck flask of step one, constant temperature is persistently stirred after 2 ~ 2.5h, obtains paraffin wax emulsions；
Step 3, paraffin wax emulsions are poured in beaker, and at least 12h is aged under room temperature；Upper strata accumulation of solids is pulled out, room temperature
It is lower to dry naturally, obtain paraffin microballoon.
The surfactant includes Triton X-100.
By polyurethane sponge as main body, be polymerized the present invention silicon rubber film on its cavernous structure surface, and utilizes stone
Wax microballoon further enhances the hydrophobicity and oleophylic performance of material.
Paraffin is the paraffin wax of higher 58 ~ 60 DEG C of fusing point.
The present invention using method be：By the regulatable porous polymer connection of the intercrossed network type surface property of the present invention
In the entrance pipe of pump, it is placed directly within oil water mixture being connected to into the porous polymer at tube inlet；It is many due to this
The hydrophobicity of Porous materials so as to can float on the water surface；When the pump is operated, the oil phase in oil water mixture, can pass through IPN
The regulatable poromeric duct of network-type surface property；Concentrated by the discharge pipe of pump and drain into containers store, be enriched with oil phase
Material；Simultaneously as the hydrophobicity of porous material itself, repels the water in oil water mixture into poromeric passage,
Water is set mutually to remain in former container；So as to the oil phase for realizing oil water mixture is separated from the water.
Regulatable porous polymer of a kind of intercrossed network type surface property that the present invention is provided and preparation method thereof, utilizes
The hydrophobicity and lipophile of silicon rubber and paraffin microballoon, with polyurethane sponge as porous material, with the paraffin microballoon of independent research
For modifying agent, preparing can carry out the detached material of continuous water-oil phase；The present invention utilizes polyurethane sponge, silicon rubber and stone
The raw materials such as wax are cheap, and preparation process is simple is pollution-free；The material to be mainly characterized by pore structure flourishing, constitute continuous being connected
Three-dimensional porous structure, specific surface area is big, to oil phase high adsorption capacity, while the addition of paraffin microballoon increased the hydrophobic of material
Property, realize continuous, the efficient separation to oil phase substance in oil water mixture；Because the continuous three-dimensional being connected is more in the present invention
If pore structure constitutes dry passage, the channel selectivity is strong, only allows oil phase to pass through, therefore the present invention and conventional water-oil separating material
Compare, be no longer limited to sorbing material own vol or adsorbance, continuously can use for a long time, process without the need for regeneration, operation
Simply, it is easy to use, and oil phase substance directly can be continuously collected, enormously simplify the removal process of oil phase substance；The present invention
The preparation method of the paraffin microballoon of middle micro-meter scale, paraffin microballoon prepared by the method increased poromeric hydrophobicity, make
Channel selectivity is high, and oil-water separation effect is further enhanced.A kind of intercrossed network type surface property controllable that the present invention is provided
Porous polymer and preparation method thereof, realize being continuously separated and reclaiming for oil phase, be remarkably improved the separative efficiency of greasy dirt with
And the efficiency of repairing environment, and preparation cost is cheap, process is simple, preparation process green non-pollution；Separate in water-oil phase and lead
Domain（Such as, oil tanker leakage etc.）In have wide practical use.
Description of the drawings
Fig. 1 is the enlarged photograph of paraffin microballoon in the present invention；
Fig. 2 is silicon rubber in the present invention/contact angle of the paraffin microsphere compound to water；
Fig. 3 is poromeric loose structure scanning electron microscope (SEM) photograph of the invention；
Fig. 4 is the microcosmic scanning electron microscope (SEM) photograph of poromeric loose structure of the invention；
Fig. 5 is silicon rubber of the present invention and paraffin microspheres quality ratio is 10：1 poromeric stress-strain test figure.
Specific embodiment
The present invention is further described below in conjunction with the accompanying drawings.
Embodiment 1：
As shown in Fig. 1 ~ 5, the regulatable porous polymer of intercrossed network type surface property, it is characterised in that：Including：Material
For the main body of porous material, the silicon rubber of be polymerized in the three-dimensional cavernous structure of the main body one layer of silicon rubber and paraffin microballoon composition
Glue/paraffin microsphere compound.
The porous material includes polyurethane sponge.
The material of the silicon rubber includes 107-2000 double component room temperature vulcanization silicon rubbers.
The manufacturer of 107-2000 double component room temperature vulcanization silicon rubbers is Jinan nation of state chemical industry.
The paraffin microballoon is the paraffin microballoon of micro-meter scale.
The regulatable poromeric preparation method of intercrossed network type surface property, it is characterised in that：Including following step
Suddenly：
S01, by main body of the material for porous material suitable size is cut into according to actual needs, is then placed in baking oven,
110oC is dried 1 hour；
S02, weighs in mass ratio silicon rubber and paraffin microballoon, and curing agent is added after stirring, then fully stirs
1min is mixed, mixed liquor is obtained；The mass ratio is silicon rubber：Paraffin microballoon=10:1；
S03, the main body in baking oven is taken out, and is put in the mixed liquor in step S02 and is fully absorbed, and is put after saturation to be absorbed
In entering baking oven, isothermal curing 2h obtains finished product.
Curing agent：Silicon rubber=1：10 weight is than adding.
The preparation method of the paraffin microballoon is comprised the following steps：
Step one, adds water and Triton X-100, in placing into 70 DEG C of thermostat water baths in three-neck flask
Heating 10min, with electric mixer 2min is stirred；The addition of the Triton X-100 is the paraffin microballoon matter
3 times of amounts of amount；
Step 2, by the paraffin wax of solid-state, plus heat fusing, form liquid paraffin；With per minute 3 drop speed, slowly
In being added drop-wise to the three-neck flask of step one, constant temperature is persistently stirred after 2h, obtains paraffin wax emulsions；
Step 3, paraffin wax emulsions are poured in beaker, and under room temperature 12h is aged；Upper strata accumulation of solids is pulled out, under room temperature certainly
So dry, obtain paraffin microballoon.
Embodiment 2：
As shown in Fig. 1 ~ 5, the regulatable porous polymer of intercrossed network type surface property, it is characterised in that：Including：Material
For the main body of porous material, the silicon rubber of be polymerized in the three-dimensional cavernous structure of the main body one layer of silicon rubber and paraffin microballoon composition
Glue/paraffin microsphere compound.
The porous material includes polyurethane sponge.
The material of the silicon rubber includes 107-2000 double component room temperature vulcanization silicon rubbers.
The manufacturer of 107-2000 double component room temperature vulcanization silicon rubbers is Jinan nation of state chemical industry.
The paraffin microballoon is the paraffin microballoon of micro-meter scale.
The regulatable poromeric preparation method of intercrossed network type surface property, it is characterised in that：Including following step
Suddenly：
S01, by main body of the material for porous material suitable size is cut into according to actual needs, is then placed in baking oven,
120oC is dried 2 hours；
S02, weighs in mass ratio silicon rubber and paraffin microballoon, and curing agent is added after stirring, then fully stirs
2min is mixed, mixed liquor is obtained；The mass ratio is silicon rubber：Paraffin microballoon=5:1；
S03, the main body in baking oven is taken out, and is put in the mixed liquor in step S02 and is fully absorbed, and is put after saturation to be absorbed
In entering baking oven, isothermal curing at least 2h obtains finished product.
Curing agent：Silicon rubber=1：10 weight is than adding.
The preparation method of the paraffin microballoon is comprised the following steps：
Step one, adds water and Triton X-100, in placing into 80 DEG C of thermostat water baths in three-neck flask
Heating 15min, with electric mixer 3min is stirred；The addition of the Triton X-100 is the paraffin microballoon matter
5 times of amounts of amount；
Step 2, by the paraffin wax of solid-state, plus heat fusing, form liquid paraffin；With per minute 5 drop speed, slowly
In being added drop-wise to the three-neck flask of step one, constant temperature is persistently stirred after 2.5h, obtains paraffin wax emulsions；
Step 3, paraffin wax emulsions are poured in beaker, and at least 12h is aged under room temperature；Upper strata accumulation of solids is pulled out, room temperature
It is lower to dry naturally, obtain paraffin microballoon.
Embodiment 3：
As shown in Fig. 1 ~ 5, the regulatable porous polymer of intercrossed network type surface property, it is characterised in that：Including：Material
For the main body of porous material, the silicon rubber of be polymerized in the three-dimensional cavernous structure of the main body one layer of silicon rubber and paraffin microballoon composition
Glue/paraffin microsphere compound.
The porous material includes polyurethane sponge.
The material of the silicon rubber includes 107-2000 double component room temperature vulcanization silicon rubbers.
The manufacturer of 107-2000 double component room temperature vulcanization silicon rubbers is Jinan nation of state chemical industry.
The paraffin microballoon is the paraffin microballoon of micro-meter scale.
The regulatable poromeric preparation method of intercrossed network type surface property, it is characterised in that：Including following step
Suddenly：
S01, by main body of the material for porous material suitable size is cut into according to actual needs, is then placed in baking oven,
115oC is dried 1.5 hours；
S02, weighs in mass ratio silicon rubber and paraffin microballoon, and curing agent is added after stirring, then fully stirs
1.5min is mixed, mixed liquor is obtained；The mass ratio is silicon rubber：Paraffin microballoon=8:1；
S03, the main body in baking oven is taken out, and is put in the mixed liquor in step S02 and is fully absorbed, and is put after saturation to be absorbed
In entering baking oven, isothermal curing at least 2h obtains finished product.
Curing agent：Silicon rubber=1：10 weight is than adding.
The preparation method of the paraffin microballoon is comprised the following steps：
Step one, adds water and surfactant in three-neck flask, places in 75 DEG C of thermostat water baths and heats
13min, with electric mixer 2.5min is stirred；The addition of the surfactant is 4 times of amounts of the paraffin microspheres quality；
Step 2, by the paraffin wax of solid-state, plus heat fusing, form liquid paraffin；With per minute 4 drop speed, slowly
In being added drop-wise to the three-neck flask of step one, constant temperature is persistently stirred after 2.2h, obtains paraffin wax emulsions；
Step 3, paraffin wax emulsions are poured in beaker, and at least 12h is aged under room temperature；Upper strata accumulation of solids is pulled out, room temperature
It is lower to dry naturally, obtain paraffin microballoon.
The surfactant includes Triton X-100.
The above is only the preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (5)
1. the regulatable porous polymer of intercrossed network type surface property, it is characterised in that：Including：Material is the master of porous material
Body, silicon rubber/paraffin microballoon that be polymerized in the three-dimensional cavernous structure of the main body one layer of silicon rubber and paraffin microballoon are constituted is combined
Thing；The material of the silicon rubber includes 107-2000 double component room temperature vulcanization silicon rubbers；The paraffin microballoon is micro-meter scale
Paraffin microballoon.
2. the regulatable porous polymer of intercrossed network type surface property according to claim 1, it is characterised in that：It is described
Porous material includes polyurethane sponge.
3. the regulatable poromeric preparation side of intercrossed network type surface property according to any one of claim 1 ~ 2
Method, it is characterised in that：Comprise the following steps：
S01, suitable size is cut into according to actual needs by material for the main body of porous material, is then placed in baking oven, 110 ~
120oC is dried 1 ~ 2 hour；
S02, weighs in mass ratio silicon rubber and paraffin microballoon, adds curing agent after stirring, then it is sufficiently stirred for 1 ~
2min, obtains mixed liquor；The mass ratio is silicon rubber：Paraffin microballoon=10 ~ 5:1；
S03, the main body in baking oven is taken out, and is put in the mixed liquor in step S02 and is fully absorbed, and baking is put into after saturation to be absorbed
In case, isothermal curing at least 2h obtains finished product.
4. the regulatable poromeric preparation method of intercrossed network type surface property according to claim 3, it is special
Levy and be：The preparation method of the paraffin microballoon is comprised the following steps：
Step one, adds water and surfactant in three-neck flask, place into heating 10 in 70 ~ 80 DEG C of thermostat water baths ~
15min, with electric mixer 2 ~ 3min is stirred；The addition of the surfactant is 3 ~ 5 times of the paraffin microspheres quality；
Step 2, by the paraffin wax of solid-state, plus heat fusing, form liquid paraffin；With the speed of per minute 3 ~ 5 drops, slow drop
In being added to the three-neck flask of step one, constant temperature is persistently stirred after 2 ~ 2.5h, obtains paraffin wax emulsions；
Step 3, paraffin wax emulsions are poured in beaker, and at least 12h is aged under room temperature；Upper strata accumulation of solids is pulled out, under room temperature certainly
So dry, obtain paraffin microballoon.
5. the regulatable poromeric preparation method of intercrossed network type surface property according to claim 4, it is special
Levy and be：The surfactant includes Triton X-100.
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| CN107474538B (en) * | 2017-07-26 | 2020-09-25 | 江苏大学 | Functional film capable of reducing gas transmission efficiency at high temperature, preparation method and application thereof |
| CN107880852A (en) * | 2017-11-16 | 2018-04-06 | 南京工程学院 | The preparation of paraffin/silicon rubber phase-change microcapsule |
| CN115322599A (en) * | 2022-08-31 | 2022-11-11 | 上海大学 | Temperature-control coating, preparation method and application thereof |
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| CN1448425A (en) * | 2003-04-14 | 2003-10-15 | 浙江大学 | Process of preparing polymer porous leg by separation and combination of paraffin microballons porous making agent and thermotropic phase |
| CN1721030A (en) * | 2005-06-09 | 2006-01-18 | 南京大学 | Super-hydrophobic/super-oleophilic oil-water separating net |
| CN102660046A (en) * | 2012-05-11 | 2012-09-12 | 北京航空航天大学 | Preparation method of superhydrophobic/superoleophilic sponge |
| CN104830367A (en) * | 2015-05-25 | 2015-08-12 | 哈尔滨工业大学 | Method for separating shale oil and water mixture by using paraffin and magnetic iron |
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2015
- 2015-08-14 CN CN201510502804.6A patent/CN105080185B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1448425A (en) * | 2003-04-14 | 2003-10-15 | 浙江大学 | Process of preparing polymer porous leg by separation and combination of paraffin microballons porous making agent and thermotropic phase |
| CN1721030A (en) * | 2005-06-09 | 2006-01-18 | 南京大学 | Super-hydrophobic/super-oleophilic oil-water separating net |
| CN102660046A (en) * | 2012-05-11 | 2012-09-12 | 北京航空航天大学 | Preparation method of superhydrophobic/superoleophilic sponge |
| CN104830367A (en) * | 2015-05-25 | 2015-08-12 | 哈尔滨工业大学 | Method for separating shale oil and water mixture by using paraffin and magnetic iron |
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