CN110423298A - A kind of water-oil separating SiO2/ polystyrene composite porous material preparation method - Google Patents
A kind of water-oil separating SiO2/ polystyrene composite porous material preparation method Download PDFInfo
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- CN110423298A CN110423298A CN201910606886.7A CN201910606886A CN110423298A CN 110423298 A CN110423298 A CN 110423298A CN 201910606886 A CN201910606886 A CN 201910606886A CN 110423298 A CN110423298 A CN 110423298A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
-
- 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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
Abstract
The present invention relates to a kind of water-oil separating SiO2/ polystyrene composite porous material preparation method, belongs to technical field of composite materials.Preparation method of the present invention the following steps are included: S1, will modified SiO2Uniform particle is scattered in the mixed liquor of styrene, crosslinking agent and emulsifier span 80, and is heated to certain temperature；S2, it is slowly added dropwise into the mixed liquor of step S1 into the aqueous solution containing potassium peroxydisulfate and potassium sulfate, dropwise addition process keeps constant mixing speed, obtains SiO2Particle cooperates with stable High Internal Phase Emulsion with emulsifier span 80；S3, the High Internal Phase Emulsion of step S2 is transferred to particular reactor relaying continuous insulation reaction 24~48 hours, until monomer reaction completely afterwards dry obtained SiO2/ polystyrene composite porous material.SiO produced by the present invention2/ polystyrene composite porous material has certain mechanical performance, and porosity is larger, is suitable as the adsorbent material of water-oil separating.
Description
Technical field
The present invention relates to a kind of technical field of composite materials, and in particular to a kind of SiO with oil-water separation2/
Polystyrene composite porous material and preparation method thereof.
Background technique
With the quickening of modernization construction, hydrocarbon pollution is more serious, and the research work in terms of water-oil separating is drawn
The attention of people is played, common oil-water separation method has gravity separation method, floatation, embrane method, absorption method, biological treatment etc..
Water-oil separating material is many kinds of, and preparation method and adsorption effect are different, and porous adsorbing material is because of its specific surface area
Greatly, the advantages that preparation is simple, adsorption efficiency is high is widely used in water-oil separating field.Patent 103157392B provides one kind can
The water-oil separating porous material preparation method of degradation will be placed in silica airsetting by mutually isolated polylactic acid film
In glue-alcohol dispersion liquid, curing and drying obtains the polylactic acid porous film of aerosil@, and material preparation is simple, can be real
Now effective water-oil separating；Patent 106110901B discloses a kind of antifouling water-oil separating material of antibacterial and preparation method thereof, will
The filter membrane material of overactivation processing immerses Cu2+In solution, stirring at normal temperature, carrying out in-situ reducing again to mixed system, to obtain antibacterial anti-
Sump oil water separation material, the preparation method is simple, good anti-bacterial effect, anti-pollution are high, separative efficiency is high, can be used for containing inorganic
The purification separation of complicated oily waste water including object, organic matter and microorganism is handled；Liu Xiaomeng etc. is by polyurethane sponge
It is mixed in alcohol solvent with the graphene oxide coated by nano silica, is not destroying polyurethane sponge inherent structure
On the basis of it is coated, obtain the Hydrophobic adsorbent material with high-specific surface area and microcellular structure, absorption test shows this
Material, which has chloroform, is equivalent to 180 times of own wt of absorption property, can be achieved with reusing by simply squeezing and
Recycling；Wang Jintao etc. uses NaClO3Solution impregnates cotton fabric and obtains a kind of super wet fabric to can be used as water-oil separating dynamic
Power drive film, the material are not only prepared simply, and water-oil separating efficiency is all larger than in acid solution, alkaline solution and salting liquid
95.7%, it can be used for Water warfare and oiliness sewage treatment.
Summary of the invention
On this basis, the present invention prepares the SiO with hierarchical porous structure using Water-In-Oil High Internal Phase Emulsion system2/
Polystyrene (PS) composite porous material has larger porosity and certain mechanical performance, to oily matters such as chloroform, n-hexanes
With certain adsorption effect, water-oil separating material can be used as.
In the present invention, a kind of water-oil separating SiO is provided2/ polystyrene composite porous material preparation method, including
Following steps:
S1, by silane coupler modified SiO2Uniform particle is scattered in styrene, crosslinking agent and emulsifier span80's
Mixed liquor, constant speed stir and are warming up to certain temperature；
S2, the aqueous solution containing potassium peroxydisulfate and potassium sulfate is added dropwise to the mixed liquor of step S1, the process that is added dropwise keeps permanent
Determine mixing speed, obtains SiO2Particle cooperates with stable High Internal Phase Emulsion with emulsifier span 80；
S3, the High Internal Phase Emulsion of step S2 is transferred to plastic material reactor relaying continuous insulation reaction 24~48 hours,
To monomer reaction completely afterwards dry obtained SiO2/ polystyrene composite porous material.
Further, in step sl, the modified SiO2Particle additive amount is the 0.1%- of styrene monomer quality
2%, preferably additive amount be styrene monomer quality 0.3%-0.5%.
Further, in step sl, the crosslinking agent is more vinyl function monomers, preferably dimethacrylate second
Diol ester or divinylbenzene.
Further, in step sl, the molar ratio of the crosslinking agent and styrene is 1:4-1:2.
Further, in step s 2, interior phase accounting is 75%-95% in the High Internal Phase Emulsion, is preferably controlled in
80%-85%.
In the present invention, a kind of SiO prepared by the above method is on the other hand additionally provided2/ polystyrene is compound porous
Material is made material and is suitable for water-oil separating.
Compared with prior art, technical solution of the present invention has the advantage that as follows: the present invention is high using Water-In-Oil
Internal phase emulsions system prepares the SiO with larger porosity2/ polystyrene composite porous material.The preparation method is with water phase
For dispersed phase, minimizing technology is simple；Continuous phase-polymerization forms the porous material with hierarchical porous structure.It is produced by the present invention porous
Material has certain mechanical performance, has certain adsorption effect to oily matters such as chloroform, n-hexanes, can be used as water-oil separating material
Material.
Detailed description of the invention
Attached drawing is only used for showing the purpose of specific embodiment, and is not to be construed as limiting the invention.
Fig. 1 a is SiO made from the embodiment of the present invention 12The scanning electron microscope (SEM) photograph of/polystyrene composite porous material；
Fig. 1 b is SiO made from the embodiment of the present invention 32The scanning electron microscope (SEM) photograph of/polystyrene composite porous material；
Fig. 1 c is SiO made from the embodiment of the present invention 52The scanning electron microscope (SEM) photograph of/polystyrene composite porous material；
Fig. 2 is difference SiO made from the embodiment of the present invention2The compression performance test chart of the composite porous material of content；
Fig. 3 is difference SiO made from the embodiment of the present invention2The composite porous material of content is bent to the absorption oil mass of organic matter
Line chart.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention
Formula is further described.
Embodiment 1
(1) 4g styrene (St), 1.2g ethylene glycol dimethacrylate (EGDMA), 1g department are added in 250ml four-hole bottle
Disk 80 (Span80) and the silane coupler modified SiO of 0.004g2Particle, the silane coupling agent are methacryloxypropyl
Trimethoxy silane, agitating and heating are warming up to 60 DEG C；
(2) 0.25g potassium peroxydisulfate (KPS) is weighed, 0.1g potassium sulfate is dissolved in 45ml deionized water；
(3) after in four-hole bottle temperature stablize after, will in (2) with solution with constant pressure funnel instillation four-hole boiling flask in,
Time for adding is 0.5h or so；
(4) it is added dropwise and continues to stir 3min, obtain the thick shape lotion of milky to get High Internal Phase Emulsion (HIPE)；
(5) High Internal Phase Emulsion is transferred in plastics column tube, is placed in drying after 60 DEG C of baking ovens react 24 hours, obtains
SiO2/ polystyrene composite porous material.
SiO made from embodiment 12The scanning electron microscope (SEM) photograph of/polystyrene composite porous material is as shown in Figure 1a.
Embodiment 2
(1) the modified SiO of 4g styrene, 1.2g EGDMA, 1g Span80 and 0.008g is added in 250ml four-hole bottle2Grain
Son, method of modifying is same as Example 1, and agitating and heating is warming up to 60 DEG C；
(2) 0.25g KPS is weighed, 0.1g potassium sulfate is dissolved in 45ml deionized water；
(3) after in four-hole bottle temperature stablize after, will in (2) with solution with constant pressure funnel instillation four-hole boiling flask in,
Time for adding is 0.5h or so；
(4) it is added dropwise and continues to stir 3min, obtain the thick shape lotion of milky to get High Internal Phase Emulsion (HIPE)；
(5) High Internal Phase Emulsion is transferred in plastics column tube, is placed in drying after 60 DEG C of baking ovens react 24 hours, obtains
SiO2/ polystyrene composite porous material.
Embodiment 3
(1) the modified SiO of 4g styrene, 1.2g EGDMA, 1g Span80 and 0.012g is added in 250ml four-hole bottle2Grain
Son, method of modifying is same as Example 1, and agitating and heating is warming up to 60 DEG C；
(2) 0.25g KPS is weighed, 0.1g potassium sulfate is dissolved in 45ml deionized water；
(3) after in four-hole bottle temperature stablize after, will in (2) with solution with constant pressure funnel instillation four-hole boiling flask in,
Time for adding is 0.5h or so；
(4) it is added dropwise and continues to stir 3min, obtain the thick shape lotion of milky to get High Internal Phase Emulsion (HIPE)；
(5) High Internal Phase Emulsion is transferred in plastics column tube, is placed in drying after 60 DEG C of baking ovens react 24 hours, obtains
SiO2/ polystyrene composite porous material.
SiO made from embodiment 32The scanning electron microscope (SEM) photograph of/polystyrene composite porous material is as shown in Figure 1 b.
Embodiment 4
(1) the modified SiO of 4g styrene, 1.2g EGDMA, 1g Span80 and 0.016g is added in 250ml four-hole bottle2Grain
Son, method of modifying is same as Example 1, and agitating and heating is warming up to 60 DEG C；
(2) 0.25g KPS is weighed, 0.1g potassium sulfate is dissolved in 45ml deionized water；
(3) after in four-hole bottle temperature stablize after, will in (2) with solution with constant pressure funnel instillation four-hole boiling flask in,
Time for adding is 0.5h or so；
(4) it is added dropwise and continues to stir 3min, obtain the thick shape lotion of milky to get High Internal Phase Emulsion (HIPE)；
(5) High Internal Phase Emulsion is transferred in plastics column tube, is placed in drying after 60 DEG C of baking ovens react 48 hours, obtains
SiO2/ polystyrene composite porous material.
Embodiment 5
(1) the modified SiO of 4g styrene, 1.2g EGDMA, 1g Span80 and 0.020g is added in 250ml four-hole bottle2Grain
Son, method of modifying is same as Example 1, and agitating and heating is warming up to 60 DEG C；
(2) 0.25g KPS is weighed, 0.1g potassium sulfate is dissolved in 45ml deionized water；
(3) after in four-hole bottle temperature stablize after, will in (2) with solution with constant pressure funnel instillation four-hole boiling flask in,
Time for adding is 0.5h or so；
(4) it is added dropwise and continues to stir 3min, obtain the thick shape lotion of milky to get High Internal Phase Emulsion (HIPE)；
(5) High Internal Phase Emulsion is transferred in plastics column tube, is placed in drying after 60 DEG C of baking ovens react 24 hours, obtains
SiO2/ polystyrene composite porous material.
SiO made from embodiment 52The scanning electron microscope (SEM) photograph of/polystyrene composite porous material is as illustrated in figure 1 c.
To SiO made from the embodiment of the present invention2/ polystyrene composite porous material carries out property representation:
As shown in Fig. 1 a, Fig. 1 b and Fig. 1 c, to porous material made from the embodiment of the present invention 1, embodiment 3 and embodiment 5
It is scanned Electronic Speculum test, the results showed that surfactant (Span80) and SiO2Synergistic stability effect make be added solids
Porous material bore hole size it is smaller.With SiO2The pore size of the increase of content, porous material is gradually reduced, and in SiO2
When content is 0.3%, hole size is more uniform, and pore-size distribution is relatively narrow, is then further added by SiO2There is hole size difference in content
The homogeneity of big phenomenon, bore hole size size is deteriorated；This may be due to SiO2Particle does not scatter well, Bu Nengyu
Surfactant cooperates with stable emulsion well, causes hole size inhomogenous.
As shown in Fig. 2, to difference made from the embodiment of the present invention 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5
SiO2Content porous material carries out compression performance test, the results showed that works as SiO2Dosage from 0.1% increase to 0.3% when, porous material
The compressive strength of material increases to 4.25MPa from 3.90MPa；With SiO2Dosage continues growing, the compressive strength of porous material and
Downward trend is all slightly presented in compression modulus；SiO2When too high levels, mechanical property relative reduction, this may be because of SiO2Grain
Sub- dosage continues to increase so that SiO2Reunite between particle, when by external force, generates stress and concentrate, porous material can be made instead
Performance is declined.
As shown in figure 3, to difference made from the embodiment of the present invention 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5
SiO2Content porous material carries out absorption property test, carries out absorption test to chloroform and n-hexane respectively, test result shows
Difference SiO made from the embodiment of the present invention2Content porous material has certain adsorptivity to oily material, to solubility parameters phase
Close substance-adsorbing is more preferable.
In the absence of conflict, the feature in embodiment and embodiment herein-above set forth can be combined with each other.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of water-oil separating SiO2/ polystyrene composite porous material preparation method, which comprises the following steps:
S1, by silane coupler modified SiO2Uniform particle is scattered in the mixed liquor of styrene, crosslinking agent and emulsifier span80
In, constant speed stirs and is warming up to certain temperature；
S2, it is added dropwise to the aqueous solution containing potassium peroxydisulfate and potassium sulfate to the mixed liquor of step S1, dropwise addition process, which is kept constant, to be stirred
Speed is mixed, SiO is obtained2Particle cooperates with stable High Internal Phase Emulsion with emulsifier span80；
S3, the High Internal Phase Emulsion of step S2 is transferred to plastic material reactor relaying continuous insulation reaction 24~48 hours, until list
Precursor reactant completely afterwards dry obtained SiO2/ polystyrene composite porous material.
2. a kind of water-oil separating SiO according to claim 12/ polystyrene composite porous material preparation method, it is special
Sign is that in step sl, silane coupling agent used is propyl front three oxosilane, three ethoxy silane of propyl, octyl trimethoxy
Silane, octyltri-ethoxysilane, methyl allyl acyloxypropyl trimethoxysilane and methacryloxypropyl triethoxy
Any one of silane.
3. a kind of water-oil separating SiO according to claim 22/ polystyrene composite porous material preparation method, it is special
Sign is that in step sl, silane coupling agent used is methyl allyl acyloxypropyl trimethoxysilane.
4. a kind of water-oil separating SiO according to claim 12/ polystyrene composite porous material preparation method, it is special
Sign is, in step sl, the silane coupler modified SiO2Particle additive amount is the 0.1%- of styrene monomer quality
2%.
5. a kind of water-oil separating SiO according to claim 42/ polystyrene composite porous material preparation method, it is special
Sign is, in step sl, the silane coupler modified SiO2Particle additive amount is the 0.3%- of styrene monomer quality
0.5%.
6. a kind of water-oil separating SiO according to claim 12/ polystyrene composite porous material preparation method, it is special
Sign is that in step sl, the crosslinking agent is more vinyl function monomers.
7. a kind of water-oil separating SiO according to claim 62/ polystyrene composite porous material preparation method, it is special
Sign is that in step sl, the crosslinking agent is ethylene glycol dimethacrylate or divinylbenzene.
8. a kind of water-oil separating SiO according to claim 12/ polystyrene composite porous material preparation method, it is special
Sign is that in step sl, the molar ratio of the crosslinking agent and styrene is 1:4-1:2.
9. a kind of water-oil separating SiO according to claim 12/ polystyrene composite porous material preparation method, it is special
Sign is that in step s 2, interior phase accounting is 75%-95% in the High Internal Phase Emulsion.
10. a kind of SiO prepared such as any one of claim 1-9 the method2/ polystyrene composite porous material, can be used for oil
Water separation.
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| CN114471486A (en) * | 2022-01-29 | 2022-05-13 | 蚌埠学院 | Super-hydrophobic silicon dioxide/polydivinylbenzene nano composite material and preparation method thereof |
| CN115215961A (en) * | 2022-08-09 | 2022-10-21 | 武汉理工大学 | Water-absorbing foam based on double emulsifiers and preparation method thereof |
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