CN105771322A - Super hydrophilic oil-water separation filter paper and preparation method thereof - Google Patents
Super hydrophilic oil-water separation filter paper and preparation method thereof Download PDFInfo
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- CN105771322A CN105771322A CN201610335002.5A CN201610335002A CN105771322A CN 105771322 A CN105771322 A CN 105771322A CN 201610335002 A CN201610335002 A CN 201610335002A CN 105771322 A CN105771322 A CN 105771322A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0414—Surface modifiers, e.g. comprising ion exchange groups
- B01D2239/0421—Rendering the filter material hydrophilic
Abstract
The invention discloses a preparation method of super hydrophilic oil-water separation filter paper. The method comprises the following steps: by a dip coating method, immersing filter paper into a solution which is formed by evenly mixing nano silicon dioxide particles, a silane coupling agent, a catalyst, absolute ethyl alcohol and deionized water; and carrying out ultrasonic dispersion, taking out and naturally drying the filter paper to obtain the super hydrophilic oil-water separation filter paper. The filter paper disclosed by the invention is simple in preparation method; the raw materials are universal and available; the stability is good; the prepared super hydrophilic oil-water separation filter paper is high in pore permeability, and can be applied to the fields of oil-water mixture separation, oily sewage treatment and the like; the separation efficiency can reach 99.5% and higher; and the industrial production and application prospect is wide.
Description
Technical field
The present invention relates to a kind of Superhydrophilic oil-water separation filter paper and preparation method thereof, belong to organo-mineral complexing technical field of function materials.
Background technology
A large amount of discharges of productive life oil-polluted water and the generation of Crude Oil at Sea leakage accident, have higher requirement to oily water separation technique and material.Oily waste water is essentially from industries such as oil exploitation, crude oil leakage, ship ballast water and chemical industry, iron and steel, food, weaving, machinings.The oil-polluted water of discharge in environment, destroys ecological balance, endangers human health, therefore oil-polluted water is carried out oil-water separation, be conducive to water purification, can also be removed the impurity such as moisture in product oil by oil-water separation, improves oil quality.
Utilize the special wellability of material to the different interface interactions of oil and water to realize oil-water separation, have become as the important breakthrough mouth promoting oily water separation technique development, compared with traditional oil-water separation material, there is special infiltrating oil-water separation material there is high efficiency and high selectivity.At present, there is special infiltrating oil-water separation material and mainly include oil removing and two classes that dewater.Utilize super-hydrophobic special wettability, can make that oil passes through and water does not pass through completely, thus efficiently separating oil water mixture, many research is had to be applied to oil-water separation by super-hydrophobic so far, oil-water separation mesh film with super-hydrophobic and super oleophylic function and preparation method thereof disclosed in Chinese patent CN1387932A, CN1721030A, CN101518695A and CN101708384A.Equally, utilize super hydrophilic special wettability, can make that water passes through and oil does not pass through completely, realizing efficiently separating of oil water mixture, Chinese patent CN105413236A, CN102974226A, CN105056770A, CN103893999A disclose the oil-water separation mesh film with super hydrophilic and superoleophobic function and preparation method thereof.
Under the premise keeping high oil-water separation efficiency, utilize versatile material, process simplification, improve stability, reduce cost, it is achieved the extensive preparation and application of oil-water separation material are the developing direction in this field.Compared with metal nethike embrane or other hard materials, paper base material has the advantage such as softness, easy shaping, and the preparation for oil-water separation material has unique advantage, but it is few for the report of oil-water separation to prepare super hydrophobic material with paper products for base material.WangSuhao etc. (Appl.Mater.Inter., 2010,2,677-683) utilize polystyrene that Nano particles of silicon dioxide sticks to ordinary filter paper surface, and the super-hydrophobic/super-oleophilic filter paper of preparation can remove the greasy dirt of floating on water.The preparation method that Chinese patent CN102225273A discloses a kind of super-hydrophobic super-oleophylic paper substrate separation material, utilizes silylating reagent that Nano particles of silicon dioxide colloidal sol is modified, and is soaked by filter paper and wherein naturally dries, obtains super-hydrophobic ultra-lipophilic paper-based separating material.And it is less to prepare the report of super hydrophilic material with paper base material, Chinese patent CN104492276A discloses the class preparation method for the oil-water separation film under strong acid, highly basic, hypersaline environment, with filter paper for supporting perforated substrate, by its hydrophilic polymer co-crosslinking with hydroxyl, obtain the filter paper nethike embrane with the hydrogel cladding of Multi-network.The problems such as the preparation method ubiquity complex process of above-mentioned oil-water separation film, complex steps, simultaneously in separating material recycling and disposal, cause certain environmental pollution, therefore seek simple and fast, that economic and environment-friendly method prepares super hydrophilic oil-water separation material is significant.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to provide a kind of Superhydrophilic oil-water separation filter paper and preparation method thereof.
The preparation method of Superhydrophilic oil-water separation filter paper of the present invention, it is adopt dip coating, by filter paper impregnation in by the mixed uniformly solution of nanometer silicon dioxide particle, silane coupler, catalyst, dehydrated alcohol and deionized water, ultrasonic disperse, then take out nature to dry, namely prepare Superhydrophilic oil-water separation filter paper；
It is characterized in that:
Described filter paper is average pore size is that the common middling speed of 1～50 micron is qualitative or quantitative filter paper；
Described mixed solution is by weight, by nanometer silicon dioxide particle: silane coupler: catalyst: dehydrated alcohol: deionized water is that 1～5:1～5:1～5:50～200:1～5 carry out Homogeneous phase mixing and make；Wherein:
Described nano silicon particle diameter is 40～60 nanometers；
The chemical structural formula of described silane coupler is RSi (OR1)3, wherein R is-CH2CH2CH2(OCH2CH2)nOH or-CH2CH2CH2(OCH2CH2)nOCH3, n=1～200；R1For-O (CH2)mCH3, m=0～9；
Described catalyst is the mixture of a kind of or its several arbitrary volume ratios in acidic catalyst hydrochloric acid, sulphuric acid, formic acid, acetic acid, lactic acid, or the mixture of a kind of or its several any weight ratios in base catalyst sodium hydroxide, potassium hydroxide, ammonia, ethamine, ethylenediamine, triethylamine；
The method of described ultrasonic disperse is: first by mixed solution ultrasonic disperse 30～60 minutes, then by filter paper impregnation wherein, continues ultrasonic disperse 3～5 minutes.
In the preparation method of above-mentioned Superhydrophilic oil-water separation filter paper: described mixed solution preferably by weight, by nanometer silicon dioxide particle: silane coupler: catalyst: dehydrated alcohol: deionized water is that 2～4:2～4:2～4:80～150:2～4 carry out Homogeneous phase mixing and make；Wherein: described silane coupler is coupling agent 4140, i.e. Polyethylene Glycol trimethoxy silicon propyl ether；Described catalyst is acidic catalyst hydrochloric acid, sulphuric acid, formic acid, acetic acid or lactic acid, or base catalyst sodium hydroxide, potassium hydroxide, ammonia, ethamine, ethylenediamine or triethylamine.
Further, in the preparation method of above-mentioned Superhydrophilic oil-water separation filter paper, described catalyst is preferably triethylamine.
The Superhydrophilic oil-water separation filter paper that preparation method of the present invention prepares.
The super hydrophilic component of its surface after utilizing the inventive method to process can form hydrated sheath with hydrone effect, suppress protein adsorption and other organic attachments, there is self-purification function, repeatable utilization, and oil water mixture can be realized quickly efficiently separate, separation efficiency can reach more than 99.5%.
Superhydrophilic oil-water separation filter paper disclosed by the invention and preparation method thereof has the following characteristics that
(1) propose that a kind of technique is simple, cost is low, the preparation method of the oil-water separation material of energy-conserving and environment-protective；
(2) utilize ordinary filter paper, obtain Superhydrophilic oil-water separation filter paper by dip coating one step, efficient and convenient；
(3) raw material components proportioning and experiment condition are easy to control, it may be achieved the preparation of a series of Superhydrophilic oil-water separation filter papers；
(4) the super hydrophilic component of its surface after treatment can form hydrated sheath with hydrone effect, it is suppressed that protein adsorption and other organic attachments, has self-purification function；
(5) filter paper after using is prone to disposal, recoverable or burning, environmental friendliness.
Detailed description of the invention
For being prone to be further appreciated by the present invention, the present invention is further elaborated for the following example.These embodiments have certain representativeness, it is impossible to include all examples, only for the present invention is clearly described, rather than restriction the scope of the present invention.
Embodiment 1
(1) with mass ratio range, by 0.5g nanometer silicon dioxide particle, 0.5mL silane coupler 4140,0.25mL triethylamine, 10mL dehydrated alcohol, the mixing of 0.5mL deionized water, ultrasonic 30min is to dispersed；
(2) by middling speed qualitative filter paper (average pore size 30～50nm) thorough impregnation in mixed liquor, ultrasonic disperse 3min.Filter paper is taken out, naturally dries, namely obtain that there is Superhydrophilic oil-water separation filter paper.
After measured: the contact angle of this filter paper and water is less than 5 °, and the contact angle with petroleum ether (boiling point 60～90 DEG C) is 152 ° under water.
(3) adopt common defecator to carry out oil-water separation, Superhydrophilic oil-water separation filter paper is folded into funnel-form and inserts in filter funnel.The ratio of petroleum ether (boiling point 60～90 DEG C) and deionized water 1:2 by volume being mixed, ultrasonic disperse becomes oil water mixture, is quickly poured in filter paper, it may be achieved oil water mixture quickly efficiently separates, and separation efficiency can reach more than 99.5%.This filter paper good stability, has self-purification function, repeatable utilization.
Embodiment 2
(1) with mass ratio range, by 0.5g nanometer silicon dioxide particle, 0.5mL silane coupler 4140,0.25mL triethylamine, 10mL dehydrated alcohol, the mixing of 0.5mL deionized water, ultrasonic 30min is to dispersed；
(2) by middling speed qualitative filter paper (average pore size 8～11nm) thorough impregnation in mixed liquor, ultrasonic disperse 5min.Filter paper is taken out, naturally dries, namely obtain that there is Superhydrophilic oil-water separation filter paper.
After measured: the contact angle of this filter paper and water is less than 5 °, and the contact angle with petroleum ether (boiling point 60～90 DEG C) is 155 ° under water.
(3) adopt common defecator to carry out oil-water separation, Superhydrophilic oil-water separation filter paper is folded into funnel-form and inserts in filter funnel.The ratio of petroleum ether (boiling point 60～90 DEG C) and deionized water 1:2 by volume being mixed, ultrasonic disperse becomes oil water mixture, is quickly poured in filter paper, it may be achieved oil water mixture quickly efficiently separates, and separation efficiency can reach more than 99.5%.This filter paper good stability, has self-purification function, repeatable utilization.
Embodiment 3
(1) with mass ratio range, by 0.5g nanometer silicon dioxide particle, 0.25mL silane coupler 4140,0.5mL triethylamine, 10mL dehydrated alcohol, the mixing of 0.5mL deionized water, ultrasonic 30min is to dispersed；
(2) by middling speed qualitative filter paper (average pore size 30～50nm) thorough impregnation in mixed liquor, ultrasonic disperse 3min.Filter paper is taken out, naturally dries, namely obtain that there is Superhydrophilic oil-water separation filter paper.
After measured: the contact angle of this filter paper and water is less than 5 °, and the contact angle with petroleum ether (boiling point 60～90 DEG C) is 150 ° under water.
(3) adopt common defecator to carry out oil-water separation, Superhydrophilic oil-water separation filter paper is folded into funnel-form and inserts in filter funnel.The ratio of petroleum ether (boiling point 60～90 DEG C) and deionized water 1:2 by volume being mixed, ultrasonic disperse becomes oil water mixture, is quickly poured in filter paper, it may be achieved oil water mixture quickly efficiently separates, and separation efficiency can reach more than 99.5%.This filter paper good stability, has self-purification function, repeatable utilization.
Embodiment 4
(1) with mass ratio range, by 0.25g nanometer silicon dioxide particle, 0.25mL silane coupler 4140,0.25mL triethylamine, 10mL dehydrated alcohol, the mixing of 0.5mL deionized water, ultrasonic 30min is to dispersed；
(2) by middling speed qualitative filter paper (average pore size 30～50nm) thorough impregnation in mixed liquor, ultrasonic disperse 3min.Filter paper is taken out, naturally dries, namely obtain that there is Superhydrophilic oil-water separation filter paper.
After measured: the contact angle of this filter paper and water is less than 5 °, and the contact angle with petroleum ether (boiling point 60～90 DEG C) is 153 ° under water.
(3) adopt common defecator to carry out oil-water separation, Superhydrophilic oil-water separation filter paper is folded into funnel-form and inserts in filter funnel.The ratio of petroleum ether (boiling point 60～90 DEG C) and deionized water 1:2 by volume being mixed, ultrasonic disperse becomes oil water mixture, is quickly poured in filter paper, it may be achieved oil water mixture quickly efficiently separates, and separation efficiency can reach more than 99.5%.This filter paper good stability, has self-purification function, repeatable utilization.
Embodiment 5
(1) with mass ratio range, by 0.5g nanometer silicon dioxide particle, 0.25mL silane coupler 4140,0.5mL triethylamine, 10mL dehydrated alcohol, the mixing of 0.5mL deionized water, ultrasonic 30min is to dispersed；
(2) by middling speed qualitative filter paper (average pore size 30～50nm) thorough impregnation in mixed liquor, ultrasonic disperse 3min.Filter paper is taken out, naturally dries, namely obtain that there is Superhydrophilic oil-water separation filter paper.
After measured: the contact angle of this filter paper and water, less than 5 °, is 157 ° with the contact angle of normal hexane under water.
(3) adopt common defecator to carry out oil-water separation, Superhydrophilic oil-water separation filter paper is folded into funnel-form and inserts in filter funnel.The ratio of normal hexane and deionized water 1:2 by volume being mixed, ultrasonic disperse becomes oil water mixture, is quickly poured in filter paper, it may be achieved oil water mixture quickly efficiently separates, and separation efficiency can reach more than 99.5%.This filter paper good stability, has self-purification function, repeatable utilization.
Embodiment 6
(1) with mass ratio range, by 0.5g nanometer silicon dioxide particle, 0.5mL silane coupler 4140,0.25mL triethylamine, 10mL dehydrated alcohol, the mixing of 0.5mL deionized water, ultrasonic 30min is to dispersed；
(2) by middling speed qualitative filter paper (average pore size 8～11nm) thorough impregnation in mixed liquor, ultrasonic disperse 5min.Filter paper is taken out, naturally dries, namely obtain that there is Superhydrophilic oil-water separation filter paper.
After measured: the contact angle of this filter paper and water, less than 5 °, is 159 ° with the contact angle of normal hexane under water.
(3) adopt common defecator to carry out oil-water separation, Superhydrophilic oil-water separation filter paper is folded into funnel-form and inserts in filter funnel.The ratio of normal hexane and deionized water 1:2 by volume being mixed, ultrasonic disperse becomes oil water mixture, is quickly poured in filter paper, it may be achieved oil water mixture quickly efficiently separates, and separation efficiency can reach more than 99.5%.This filter paper good stability, has self-purification function, repeatable utilization.
Claims (4)
1. the preparation method of a Superhydrophilic oil-water separation filter paper, it is adopt dip coating, by filter paper impregnation in by the mixed uniformly solution of nanometer silicon dioxide particle, silane coupler, catalyst, dehydrated alcohol and deionized water, ultrasonic disperse, then take out nature to dry, namely prepare Superhydrophilic oil-water separation filter paper；
It is characterized in that:
Described filter paper is average pore size is that the common middling speed of 1～50 micron is qualitative or quantitative filter paper；
Described mixed solution is by weight, by nanometer silicon dioxide particle: silane coupler: catalyst: dehydrated alcohol: deionized water is that 1～5:1～5:1～5:50～200:1～5 carry out Homogeneous phase mixing and make；Wherein:
Described nano silicon particle diameter is 40～60 nanometers；
The chemical structural formula of described silane coupler is RSi (OR1)3, wherein R is-CH2CH2CH2(OCH2CH2)nOH or-CH2CH2CH2(OCH2CH2)nOCH3, n=1～200；R1For-O (CH2)mCH3, m=0～9；
Described catalyst is the mixture of a kind of or its several arbitrary volume ratios in acidic catalyst hydrochloric acid, sulphuric acid, formic acid, acetic acid, lactic acid, or the mixture of a kind of or its several any weight ratios in base catalyst sodium hydroxide, potassium hydroxide, ammonia, ethamine, ethylenediamine, triethylamine；
The method of described ultrasonic disperse is: first by mixed solution ultrasonic disperse 30～60 minutes, then by filter paper impregnation wherein, continues ultrasonic disperse 3～5 minutes.
2. the preparation method of Superhydrophilic oil-water separation filter paper according to claim 1, it is characterized in that: described mixed solution is by weight, by nanometer silicon dioxide particle: silane coupler: catalyst: dehydrated alcohol: deionized water is that 2～4:2～4:2～4:80～150:2～4 carry out Homogeneous phase mixing and make；Wherein: described silane coupler is coupling agent 4140, i.e. Polyethylene Glycol trimethoxy silicon propyl ether；Described catalyst is acidic catalyst hydrochloric acid, sulphuric acid, formic acid, acetic acid or lactic acid, or base catalyst sodium hydroxide, potassium hydroxide, ammonia, ethamine, ethylenediamine or triethylamine.
3. the preparation method of Superhydrophilic oil-water separation filter paper according to claim 3, it is characterised in that: described catalyst is triethylamine.
4. the Superhydrophilic oil-water separation filter paper that preparation method described in claim 1,2 or 3 prepares.
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| CN106283851A (en) * | 2016-08-08 | 2017-01-04 | 山东交通学院 | A kind of graphene oxide modification oil-water separation filter paper and preparation method thereof |
| CN106320087A (en) * | 2016-08-27 | 2017-01-11 | 安阳华森纸业有限责任公司 | Preparation method of aperture-adjustable filter paper for ion adsorption |
| CN106868948A (en) * | 2017-02-23 | 2017-06-20 | 山东交通学院 | A kind of filter paper and its simple method for preparing and application with oil-water separating function |
| CN106902645A (en) * | 2017-02-15 | 2017-06-30 | 山东工业陶瓷研究设计院有限公司 | A kind of preparation method of the super hydrophilic ceramic membrane with photocatalysis performance |
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| CN106868948A (en) * | 2017-02-23 | 2017-06-20 | 山东交通学院 | A kind of filter paper and its simple method for preparing and application with oil-water separating function |
| CN108654576A (en) * | 2018-06-15 | 2018-10-16 | 山东交通学院 | It is a kind of that there is antifouling and Dye Adsorption function water-oil separating material and preparation method thereof |
| CN109289251A (en) * | 2018-11-26 | 2019-02-01 | 北京揽山环境科技股份有限公司 | A kind of water-oil separating combined type filtering material and preparation method thereof |
| CN109289251B (en) * | 2018-11-26 | 2024-04-05 | 北京揽山环境科技股份有限公司 | Oil-water separation composite filter material and preparation method thereof |
| CN110025985A (en) * | 2019-04-25 | 2019-07-19 | 南昌航空大学 | It is a kind of to prepare oil-water separation filter paper super hydrophilic oleophobic treatment agent and its application method |
| CN110025985B (en) * | 2019-04-25 | 2021-05-25 | 南昌航空大学 | Super-hydrophilic oil-repellent treatment agent for preparing oil-water separation filter paper and using method thereof |
| CN112982030A (en) * | 2021-02-04 | 2021-06-18 | 西安理工大学 | Preparation method of super-hydrophilic/underwater super-oleophobic filter paper |
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