CN102085459A - Method for preparing anti-polluting oil-water separation ultra-filtration membrane - Google Patents
Method for preparing anti-polluting oil-water separation ultra-filtration membrane Download PDFInfo
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Abstract
The invention discloses a method for preparing an anti-polluting efficient oil-water separation ultra-filtration membrane, which comprises the following steps of: dissolving 16.0 mass percent of cellulose acetate into an N,N-dimethyl formamide solvent based on 100 percent of the mass of membrane casting solution, adding 15.0 to 30.0 mass percent of ethyl orthosilicate, and scraping a nascent state membrane with thickness of 240 microns on a glass plate; placing the nascent state membrane in the air for 10 to 30 seconds, and then soaking the nascent state membrane into gel baths of 25 DEG C, wherein the gel baths are aqueous solution of hydrochloric acid and aqueous solution of sodium hydroxide respectively; and taking out the membrane from the gel bath, placing the membrane into deionized water, and changing the water once every 5 hours to obtain the CA(TEOS)-HCl and CA(TEOS)-NaOH modified ultra-filtration membrane. The method is simple in process and mild in conditions; and the flux of the modified membrane is greatly improved, good anti-polluting performance is kept, and the modified membrane has high interception rate and can be used for treating oil-containing wastewater.
Description
Technical field
The present invention relates to a kind of preparation method of antipollution water-oil separating milipore filter.Belong to the milipore filter technology of preparing.
Background technology
The processing of oily waste water is to have become a global environmental protection difficult problem day by day.The oily waste water wide material sources, complicated component.According to statistics, contain about 300,000 tons altogether in crude oil and goods thereof in the annual waste water of discharging of oil field, the whole world, oil plant and petrochemical plant.About 1,300,000 tons altogether in industry used oil and automobile waste oil.The whole world can reach 1,000,000 tons with the oil that these waste water enter the ocean every year.Oily waste water mainly comprises oil slick, dispersed oil, oil emulsion, dissolved oil and oil-solids five classes.
As new and effective platform technology, membrane technology is being brought into play important effect at aspects such as energy-saving and emission-reduction, green manufacturing, water resource utilization, new energy development, environmental protection, biological medicines.Ultra-filtration process is comparatively ripe membrane technology, its pore diameter range is 1～100nm, realize that based on screening mechanism system separates, relatively large disposal ability is arranged, also have the operating condition gentleness simultaneously, outstanding advantages such as treating capacity is big, selectivity is high, energy consumption is low, easy amplification, demonstrate powerful development potentiality in the water-oil separating field day by day.
Milipore filter material and filming technology are the main factors of decision water-oil separating performance, and therefore selecting suitable membrane material and suitable modification filming technology is the key that realizes the separation task.Existing macromolecule member material roughly can be divided into two classes according to its hydrophilic and hydrophobic: a class is the hydrophobic film material, hydrophobic film commonly used has polyethylene, polyvinylidene fluoride and polytetrafluoroethylene (PTFE), polysulfones/polyether sulfone, polyether sulfone, cellulose ester, polysulfones, polyacrylonitrile etc.Hydrophobic film mechanical strength height, it is little influenced by surfactant, the hydrophilic membrane power consumption is low relatively, and initial flux is higher, is beneficial to water-oil separating, but because the hydrophilic ability of hydrophobic film material, can not form on the film surface and hinder " hydrated sheath " that oil droplet arrives the film surface effectively, cause a large amount of being adsorbed on the film surface of oil droplet and other impurity, film is seriously polluted, the flux decay is fast, and film is difficult to clean.Another kind of is the hydrophilic film material, for example cellulose with and various derivative, polyvinyl alcohol etc., though the film that good hydrophilicity helps reducing in the operating process pollutes, hydrophily is too high but then, film easily dissolves, can reduce the mutual diffusion of solvent and non-solvent in the inversion of phases process in the film forming procedure, thereby cause the film epidermal area blocked up, porosity is low, flux is extremely low, is not suitable for actual industrial applications.Therefore, in film-forming process, adopt certain means that the hydrophilic film material is carried out modification, when keeping its good contamination resistance, increase substantially its processing flux and be widely used in water-oil separating for milipore filter and seem most important.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of anti-pollution high-efficiency water-oil separating milipore filter, this procedure is simple, with the milipore filter of the method preparation, has the oily waste water processing flux that significantly improves and higher rejection.
A kind of preparation method of anti-pollution high-efficiency water-oil separating milipore filter is characterized in that:
This method may further comprise the steps:
(1) by casting solution quality 100, solvent N, dinethylformamide dissolve the cellulose acetate of 16.0% quality, after being stirred to homogeneous solution, add ethyl orthosilicate, mass fraction is 15.0～30.0%, stirs 5h to transparent limpid homogeneous phase casting solution down at 60 ℃; Deaeration;
(2) get clean simple glass plate, self-control scraper, lie against on the desktop, after the absolute ethyl alcohol scouring, from thermostatic bath, take out casting solution, after treating that casting solution is cooled to room temperature fully, on glass plate one end, at the uniform velocity the horizontal drawing scraper scrapes the thick nascent state film of 240 μ m to the glass plate other end on glass plate with the casting solution curtain coating;
(3) after the striking of nascent state film, in air, place after 10～30 seconds and immerse 25 ℃ coagulation bath again; Coagulation bath adopts the aqueous hydrochloric acid solution of pH=2 and the sodium hydrate aqueous solution of pH=13 respectively, and the catalysis teos hydrolysis generates nano SiO 2 particle;
(4) behind the inversion of phases freezing film, film is taken out from coagulation bath, place deionized water, every 5h changes water one time, obtains CA (TEOS)-HCl and CA (TEOS)-NaOH modified ultrafiltration membrane.
The preparation method of described efficient antipollution water-oil separating milipore filter is characterized in that can be used for efficient (high flux, high selectivity) processing of oily waste water.
The invention has the advantages that: the film preparation process is simple, mild condition.Generated in-situ inorganic nano silica dioxide granule has improved the flux of CAM significantly as pore-foaming agent, and has good oil rub resistance metachromia energy and higher oil droplet rejection (up to 99.8%).
The specific embodiment
Embodiment 1
Take by weighing 3.2g CA and 10.8g solvent N, dinethylformamide is put into there-necked flask, puts into stirring and dissolving 1h under 60 ℃ of water-bath 900r/min rotating speeds, takes by weighing the 6.0g ethyl orthosilicate then, stirs 5h down to transparent limpid homogeneous phase casting solution at 60 ℃; After stirring casting solution is left standstill 5～7h under 60 ℃, remove the bubble in the casting solution; Get clean simple glass plate, self-control scraper, lie against on the desktop, after the absolute ethyl alcohol scouring, from thermostatic bath, take out casting solution, after treating that casting solution is cooled to room temperature fully, on glass plate one end, at the uniform velocity the horizontal drawing scraper scrapes the thick nascent state film of about 240 μ m to the glass plate other end on glass plate with the casting solution curtain coating; After the striking of nascent state film, in air, place after 10～30 seconds and immerse about 25 ℃ coagulation bath again.Coagulation bath adopts aqueous hydrochloric acid solution (pH=2) respectively.Behind the inversion of phases freezing film, film is taken out from coagulation bath, place deionized water, every 5h changes water one time, obtains CA (TEOS)-HCl-30% modified ultrafiltration membrane.
Prepared CA (TEOS)-HCl-30% modified ultrafiltration membrane is through thermogravimetric analysis, scanning electron microscope analysis, contact angle is analyzed and X-ray diffraction analysis, film pore-forming performance is good, fenestra is evenly distributed, a generated in-situ nanometer silicon dioxide particle part is diffused in the coagulation bath as pore-foaming agent, and rest parts is in film surface enrichment, good hydrophilic property.The pure water flux of this film is by original blank CA membrane flux (1.7L/m
2H) be increased to about 436.9L/m
2H, when being used for water-oil separating (900ppm oil-water emulsion simulated system), processing flux can maintain 118L/m
2About h, rejection is 99.8%, has the flux response rate up to 91.7% after washed with de-ionized water, and flux still is in higher level after circular flow repeatedly.
Embodiment 2
Take by weighing 3.2g CA and 10.8g solvent N, dinethylformamide is put into there-necked flask, puts into stirring and dissolving 1h under 60 ℃ of water-bath 900r/min rotating speeds, takes by weighing the 6.0g ethyl orthosilicate then, stirs 5h down to transparent limpid homogeneous phase casting solution at 60 ℃; After stirring casting solution is left standstill 5～7h under 60 ℃, remove the bubble in the casting solution; Get clean simple glass plate, self-control scraper, lie against on the desktop, after the absolute ethyl alcohol scouring, from thermostatic bath, take out casting solution, after treating that casting solution is cooled to room temperature fully, on glass plate one end, at the uniform velocity the horizontal drawing scraper scrapes the thick nascent state film of about 240 μ m to the glass plate other end on glass plate with the casting solution curtain coating; After the striking of nascent state film, in air, place after 10～30 seconds and immerse about 25 ℃ coagulation bath again.Coagulation bath adopts sodium hydrate aqueous solution (pH=13) respectively.Behind the inversion of phases freezing film, film is taken out from coagulation bath, place deionized water, every 5h changes water one time, obtains CA (TEOS)-NaOH-30% modified ultrafiltration membrane.
Prepared CA (TEOS)-NaOH-30% modified ultrafiltration membrane is through thermogravimetric analysis, scanning electron microscope analysis, contact angle is analyzed and X-ray diffraction analysis, film pore-forming performance is good, fenestra is evenly distributed, a generated in-situ nanometer silicon dioxide particle part is diffused in the coagulation bath as pore-foaming agent, and rest parts is in film surface enrichment, good hydrophilic property.The pure water flux of this film is by original blank CA membrane flux (1.7L/m
2H) be increased to about 332.0L/m
2H, when being used for water-oil separating (900ppm oil-water emulsion simulated system), processing flux can maintain 112L/m
2About h, rejection is 99.8%, has the flux response rate up to 91.5% after washed with de-ionized water, and flux still is in higher level after circular flow repeatedly.
Embodiment 3
Take by weighing 3.2g CA and 12.8g solvent N, dinethylformamide is put into there-necked flask, puts into stirring and dissolving 1h under 60 ℃ of water-bath 900r/min rotating speeds, takes by weighing the 4.0g ethyl orthosilicate then, stirs 5h down to transparent limpid homogeneous phase casting solution at 60 ℃; After stirring casting solution is left standstill 5～7h under 60 ℃, remove the bubble in the casting solution; Get clean simple glass plate, self-control scraper, lie against on the desktop, after the absolute ethyl alcohol scouring, from thermostatic bath, take out casting solution, after treating that casting solution is cooled to room temperature fully, on glass plate one end, at the uniform velocity the horizontal drawing scraper scrapes the thick nascent state film of about 240 μ m to the glass plate other end on glass plate with the casting solution curtain coating; After the striking of nascent state film, in air, place after 10～30 seconds and immerse about 25 ℃ coagulation bath again.Coagulation bath adopts aqueous hydrochloric acid solution (pH=2) respectively.Behind the inversion of phases freezing film, film is taken out from coagulation bath, place deionized water, every 5h changes water one time, obtains CA (TEOS)-HCl-20% modified ultrafiltration membrane.
Prepared CA (TEOS)-HCl-20% modified ultrafiltration membrane is through thermogravimetric analysis, scanning electron microscope analysis, contact angle is analyzed and X-ray diffraction analysis, film pore-forming performance is good, fenestra is evenly distributed, a generated in-situ nanometer silicon dioxide particle part is diffused in the coagulation bath as pore-foaming agent, and rest parts is in film surface enrichment, good hydrophilic property.The pure water flux of this film is by original blank CA membrane flux (1.7L/m
2H) be increased to about 268.0L/m
2H, when being used for water-oil separating (900ppm oil-water emulsion simulated system), processing flux can maintain 110L/m
2About h, rejection is 99.9%, has the flux response rate up to 91.3% after washed with de-ionized water, and flux still is in higher level after circular flow repeatedly.
Embodiment 4
Take by weighing 3.2g CA and 12.8g solvent N, dinethylformamide is put into there-necked flask, puts into stirring and dissolving 1h under 60 ℃ of water-bath 900r/min rotating speeds, takes by weighing the 4.0g ethyl orthosilicate then, stirs 5h down to transparent limpid homogeneous phase casting solution at 60 ℃; After stirring casting solution is left standstill 5～7h under 60 ℃, remove the bubble in the casting solution; Get clean simple glass plate, self-control scraper, lie against on the desktop, after the absolute ethyl alcohol scouring, from thermostatic bath, take out casting solution, after treating that casting solution is cooled to room temperature fully, on glass plate one end, at the uniform velocity the horizontal drawing scraper scrapes the thick nascent state film of about 240 μ m to the glass plate other end on glass plate with the casting solution curtain coating; After the striking of nascent state film, in air, place after 10～30 seconds and immerse about 25 ℃ coagulation bath again.Coagulation bath adopts sodium hydrate aqueous solution (pH=13) respectively.Behind the inversion of phases freezing film, film is taken out from coagulation bath, place deionized water, every 5h changes water one time, obtains CA (TEOS)-NaOH-30% modified ultrafiltration membrane.
Prepared CA (TEOS)-NaOH-30% modified ultrafiltration membrane is through thermogravimetric analysis, scanning electron microscope analysis, contact angle is analyzed and X-ray diffraction analysis, film pore-forming performance is good, fenestra is evenly distributed, a generated in-situ nanometer silicon dioxide particle part is diffused in the coagulation bath as pore-foaming agent, and rest parts is in film surface enrichment, good hydrophilic property.The pure water flux of this film is by original blank CA membrane flux (1.7L/m
2H) be increased to about 195.7L/m
2H, when being used for water-oil separating (900ppm oil-water emulsion simulated system), processing flux can maintain 112L/m
2About h, rejection is 99.8%, has the flux response rate up to 94.1% after washed with de-ionized water, and flux still is in higher level after circular flow repeatedly.
Embodiment 5
Take by weighing 3.2g CA and 13.8g solvent N, dinethylformamide is put into there-necked flask, puts into stirring and dissolving 1h under 60 ℃ of water-bath 900r/min rotating speeds, takes by weighing the 3.0g ethyl orthosilicate then, stirs 5h down to transparent limpid homogeneous phase casting solution at 60 ℃; After stirring casting solution is left standstill 5～7h under 60 ℃, remove the bubble in the casting solution; Get clean simple glass plate, self-control scraper, lie against on the desktop, after the absolute ethyl alcohol scouring, from thermostatic bath, take out casting solution, after treating that casting solution is cooled to room temperature fully, on glass plate one end, at the uniform velocity the horizontal drawing scraper scrapes the thick nascent state film of about 240 μ m to the glass plate other end on glass plate with the casting solution curtain coating; After the striking of nascent state film, in air, place after 10～30 seconds and immerse about 25 ℃ coagulation bath again.Coagulation bath adopts aqueous hydrochloric acid solution (pH=2) respectively.Behind the inversion of phases freezing film, film is taken out from coagulation bath, place deionized water, every 5h changes water one time, obtains CA (TEOS)-HCl-15% modified ultrafiltration membrane.
Prepared CA (TEOS)-HCl-10% modified ultrafiltration membrane is through thermogravimetric analysis, scanning electron microscope analysis, contact angle is analyzed and X-ray diffraction analysis, film pore-forming performance is good, fenestra is evenly distributed, a generated in-situ nanometer silicon dioxide particle part is diffused in the coagulation bath as pore-foaming agent, and rest parts is in film surface enrichment, good hydrophilic property.The pure water flux of this film is by original blank CA membrane flux (1.7L/m
2H) be increased to about 150.3L/m
2H, when being used for water-oil separating (900ppm oil-water emulsion simulated system), processing flux can maintain 110L/m
2About h, rejection is 99.9%, has the flux response rate up to 97.4% after washed with de-ionized water, and flux still is in higher level after circular flow repeatedly.
Embodiment 6
Take by weighing 3.2g CA and 13.8g solvent N, dinethylformamide is put into there-necked flask, puts into stirring and dissolving 1h under 60 ℃ of water-bath 900r/min rotating speeds, takes by weighing the 3.0g ethyl orthosilicate then, stirs 5h down to transparent limpid homogeneous phase casting solution at 60 ℃; After stirring casting solution is left standstill 5～7h under 60 ℃, remove the bubble in the casting solution; Get clean simple glass plate, self-control scraper, lie against on the desktop, after the absolute ethyl alcohol scouring, from thermostatic bath, take out casting solution, after treating that casting solution is cooled to room temperature fully, on glass plate one end, at the uniform velocity the horizontal drawing scraper scrapes the thick nascent state film of about 240 μ m to the glass plate other end on glass plate with the casting solution curtain coating; After the striking of nascent state film, in air, place after 10～30 seconds and immerse about 25 ℃ coagulation bath again.Coagulation bath adopts sodium hydrate aqueous solution (pH=13) respectively.Behind the inversion of phases freezing film, film is taken out from coagulation bath, place deionized water, every 5h changes water one time, obtains CA (TEOS)-NaOH-15% modified ultrafiltration membrane.
Prepared CA (TEOS)-NaOH-15% modified ultrafiltration membrane is through thermogravimetric analysis, scanning electron microscope analysis, contact angle is analyzed and X-ray diffraction analysis, film pore-forming performance is good, fenestra is evenly distributed, a generated in-situ nanometer silicon dioxide particle part is diffused in the coagulation bath as pore-foaming agent, and rest parts is in film surface enrichment, good hydrophilic property.The pure water flux of this film is by original blank CA membrane flux (1.7L/m
2H) be increased to about 161.8L/m
2H, when being used for water-oil separating (900ppm oil-water emulsion simulated system), processing flux can maintain 104L/m
2About h, rejection is 99.8%, has the flux response rate up to 100% after washed with de-ionized water, and flux still is in higher level after circular flow repeatedly.
Comparative Examples 1
Take by weighing 3.2g CA and 16.8g solvent N, dinethylformamide is put into there-necked flask, puts under 60 ℃ of water-bath 900r/min rotating speeds stirring and dissolving 5h to transparent limpid homogeneous phase casting solution; After stirring casting solution is left standstill 5～7h under 60 ℃, remove the bubble in the casting solution; Get clean simple glass plate, self-control scraper, lie against on the desktop, after the absolute ethyl alcohol scouring, from thermostatic bath, take out casting solution, after treating that casting solution is cooled to room temperature fully, on glass plate one end, at the uniform velocity the horizontal drawing scraper scrapes the thick nascent state film of about 240 μ m to the glass plate other end on glass plate with the casting solution curtain coating; After the striking of nascent state film, in air, place after 10～30 seconds and immerse again in about 25 ℃ gel bath water.Behind the inversion of phases freezing film, film is taken out from coagulation bath, place deionized water, every 5h changes water one time, obtains the blank milipore filter of CA.
The thermogravimetric analysis of the blank milipore filter process of prepared CA, scanning electron microscope analysis, contact angle analysis and X-ray diffraction analysis, film pore-forming poor performance, porosity is low, good hydrophilic property.The pure water flux of this film is 1.7L/m
2H, when being used for water-oil separating (900ppm oil-water emulsion simulated system), processing flux can maintain 1.7L/m
2About h, rejection is 99.8%, and antifouling property is good.
Table 1 is depicted as the prepared film 1 of embodiment, film 2, film 3, film 4, film 5, the stalling characteristic of the ultra-filtration and separation 900ppm oil-water emulsion of film 6 and Comparative Examples one prepared film 7.
Table 1
Claims (1)
1. the preparation method of an antipollution water-oil separating milipore filter is characterized in that:
This method may further comprise the steps:
(1) by casting solution quality 100, solvent N, dinethylformamide dissolve the cellulose acetate of 16.0% quality, after being stirred to homogeneous solution, add ethyl orthosilicate, mass fraction is 15.0～30.0%, stirs 5h to transparent limpid homogeneous phase casting solution down at 60 ℃; Deaeration;
(2) get clean simple glass plate, self-control scraper, lie against on the desktop, after the absolute ethyl alcohol scouring, from thermostatic bath, take out casting solution, after treating that casting solution is cooled to room temperature fully, on glass plate one end, at the uniform velocity the horizontal drawing scraper scrapes the thick nascent state film of 240 μ m to the glass plate other end on glass plate with the casting solution curtain coating;
(3) after the striking of nascent state film, in air, place after 10～30 seconds and immerse 25 ℃ coagulation bath again; Coagulation bath adopts the aqueous hydrochloric acid solution of pH=2 and the sodium hydrate aqueous solution of pH=13 respectively, and the catalysis teos hydrolysis generates nano SiO 2 particle;
(4) behind the inversion of phases freezing film, film is taken out from coagulation bath, place deionized water, every 5h changes water one time, obtains CA (TEOS)-HCl and CA (TEOS)-NaOH modified ultrafiltration membrane.
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