CN106334543A - Method for preparing three-dimensional porous oil absorption material - Google Patents
Method for preparing three-dimensional porous oil absorption material Download PDFInfo
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- CN106334543A CN106334543A CN201611007945.1A CN201611007945A CN106334543A CN 106334543 A CN106334543 A CN 106334543A CN 201611007945 A CN201611007945 A CN 201611007945A CN 106334543 A CN106334543 A CN 106334543A
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- oil absorption
- absorption material
- dimensional porous
- porous oil
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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
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
-
- 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
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention relates to a method for preparing a three-dimensional porous oil absorption material. The method comprises the steps that polylactic acid is dissolved in a solvent and stirred to be dissolved, and a polylactic acid solution is obtained; under the stirring condition, a poor solvent is dropwise added into the polylactic acid solution till the solution turns turbid from clear, still standing is carried out at room temperature, replacement and vacuum drying are carried out, and the three-dimensional porous oil absorption material is obtained; or under the stirring condition, natural fibers are added into the polylactic acid solution, then the poor solvent is dropwise added till the solution phase is separated, still standing is carried out at room temperature, replacement is carried out, and the three-dimensional porous oil absorption material is obtained. The novel oil absorption material is controllable in aperture size and shape and can be suitable for different application occasions.
Description
Technical field
The invention belongs to the preparation field of oil absorption material, particularly to a kind of preparation method of three-dimensional porous oil absorption material.
Background technology
With industrial fast development, people's exploitation, transport, using and storage oil during oil leak thing can occur
Therefore, thus leading to the water resource pollution problem such as river, ocean increasingly severe.Oil pollution is to the destruction of environment and to the mankind
Harm caused the extensive concern of people, the greasy dirt revealed on the water surface must timely and effectively be removed.Commonly use at present
Oily waste treatment material includes the strong powder inorganic mineral of porous, adsorptivity, nanoscale composite film material and polypropylene melt-blown no
Spin cloth.
The Chinese patent application of Publication No. cn105214602a disclose a kind of porous oil-absorbing material and its preparation and again
Generation method, the oil absorption material preparing gained has stronger oil absorption, but its porosity only has 40%, and needs surface modification
Process, complex process, relatively costly.The Chinese patent application of Publication No. cn103772627a discloses a kind of polyacrylic acid
The preparation method of ester/lignin compound oil absorption material, the oil absorption material oil absorption of the method preparation is high, and structural homogeneity is good,
But it can only part biological degraded.
For the deficiency of foregoing invention, this invention address that the suction of high porosity, fast absorbing oil and fully biodegradable
The preparation of light wood material.
Content of the invention
The technical problem to be solved is to provide a kind of preparation method of three-dimensional porous oil absorption material, system of the present invention
Standby three-dimensional porous oil absorption material has raw material sources extensively, process is simple, porosity is high, swelling rate is fast, biodegradable,
Reusable the advantages of.
A kind of preparation method of the three-dimensional porous oil absorption material of the present invention, comprising:
(1) particles of polylactic acid is dissolved in a solvent, under normal temperature and pressure conditionses, magnetic agitation dissolves, and obtains polylactic acid
Solution；
(2) under normal temperature and pressure, stirring condition, extremely molten by being added dropwise over poor solvent in the PLA solution of step (1)
Liquid is become cloudy (reaching cloud point) by clarification, and room temperature stands, and displacement is vacuum dried under room temperature, obtains three-dimensional porous oil absorption material；
Or under agitation, natural fiber will be added in the PLA solution of step (1), be then added dropwise over bad molten
Agent is separated to solution, room temperature standing under room temperature, and displacement obtains final product three-dimensional porous oil absorption material.
The molecular weight 6.0 × 10 of polylactic acid in described step (1)4～1.0 × 105g/mol；Solvent is dichloromethane.
In described step (1), the mass percentage concentration of PLA solution is 10%～20%.
In described step (2) poor solvent be one of acetone, dehydrated alcohol, absolute methanol, normal hexane, hexamethylene or
Several.
The volume ratio of the poor solvent in the solvent in step (1) and step (2) is 1:0.5～1:1.5.
In described step (2), natural fiber is one or more of bombax cotton, Radix Calotropis giganteae fibre.
In natural fiber and polylactic acid blend system in step (2), the quality of polylactic acid is 395mg, natural fiber with poly-
The mass ratio of lactic acid is 1:10～1:2 (i.e. bombax cotton/polylactic acid=1:10～1:2；Radix Calotropis giganteae fibre/polylactic acid=1:10
～1:2).
In described step (2), natural fiber is big lumen natural fiber, and the length of natural fiber is 0.2mm～5mm.
In described step (2), room temperature time of repose is 10-24h；
Being replaced into methanol replacement in described step (2), particularly as follows: being immersed in absolute methanol, being placed in vibration on shaking table
Displace dichloromethane, change a methanol solution every 12h～24h, change 1-5 time.
Beneficial effect
(1) the novel oil absorption material of present invention preparation have raw material sources extensively, process is simple；Porosity is high, oil absorption
Greatly, swelling rate is fast；Fully biodegradable, reusable the advantages of；
(2) porosity of the three-dimensional porous oil absorption material of the present invention up to 80%～90%, water contact angle is 141.1 ° ±
10, oil absorption is 13g/g～18g/g；
(3) the novel oil absorption material pore size that the present invention makes is controlled, and controlled shape is applicable to different application field
Close, pore size can be controlled by adjusting process parameter and polymer property, such as phase separation temperature, dwell temperature, no
The parameters such as good solvent species, polymer molecular weight and polymer concentration；The shape of porous material can be by different moulds
Shape is controlling；This oil absorption material can be widely applied to the process of marine oil spill accident, and oil-water separation is processed and containing oil
The many-sides such as the process of dirty industrial wastewater.
Brief description
Fig. 1 is a kind of preparation flow schematic diagram of present invention novel three-dimensional porous oil-absorbing material；
Fig. 2 is the scanning electron microscope (SEM) photograph of three-dimensional porous oil absorption material, and wherein a is the polylactic acid porous material of embodiment 1, and b is
The big lumen natural fiber composite porous material of the polylactic acid of embodiment 2/short, c is the big lumen of the polylactic acid/length of embodiment 3
Natural fiber composite porous material；
Fig. 3 is three-dimensional porous fast oil-absorption material oil-water separation figure.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content of present invention instruction, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
With reference to the detection of fz/t 01130-2016 non-weaving cloth oil absorbency and the standard of evaluation, take compound porous oil suction
Material shape sample size is 5mm × 5mm × 5mm, and weighs, and is designated as m0；Then sample is immersed in vegetable oil at room temperature,
Take out sample after 15min, be placed on rustless steel mesh screen, allow after its 60s that naturally hangs down, be re-weighed, be designated as m1；According to following equation
Calculate oil absorption, unit is g/g；Each sample repeats above operation and averages for 3 times, as oil absorption.
Embodiment 1
(1) weigh 0.395g particles of polylactic acid respectively with me104e prunus mume (sieb.) sieb.et zucc. Teller-Tuo Li electronic balance, be dissolved in 2ml dichloro
In methane, at ambient temperature, it is allowed to be stirred well to and is completely dissolved, obtain the PLA solution that concentration is 13%.
(2) by the PLA solution having configured, under the stirring of magnetic stirring apparatuss, dropwise Deca 3ml poor solvent is extremely molten
Liquid becomes muddy by clarification, and room temperature stands 24h, takes out, is immersed in absolute methanol, is placed in vibration on shaking table, changes repeatedly
Afterwards, it is vacuum dried under room temperature, obtain three-dimensional porous material.
(3) test the oil absorbency of this three-dimensional porous material, this porosity of porous material is 90%, water contact angle is
141.7 °, oil absorption is 13g/g.
(4) by the porous material after oil suction, it is immersed in dehydrated alcohol, vibration, displaces the fluid of absorption, be dried, weight
Relapse oily 5 times afterwards, the oil absorption of this porous material is 10g/g, therefore has preferable reusability.
Embodiment 2
(1) weigh 0.395g particles of polylactic acid respectively with me104e prunus mume (sieb.) sieb.et zucc. Teller-Tuo Li electronic balance, be dissolved in 2ml dichloro
In methane, at ambient temperature, it is allowed to be stirred well to and is completely dissolved, obtain the PLA solution that concentration is 13%.
(2) by the PLA solution having configured, under the stirring of magnetic stirring apparatuss, 0.07g length is added to obtain for 0.2mm wooden
Cotton fiber, stirs, and dropwise to solution to being separated, room temperature stands 24h to Deca 3ml poor solvent, takes out, is immersed in anhydrous
In methanol, it is placed in vibration on shaking table, after changing repeatedly, is vacuum dried under room temperature, obtain polylactic acid/kapok chopped fiber and be combined
Porous material.
(3) test the oil absorbency of this composite porous material, the porosity of this porous material is 84.7%, and water contact angle is
141.4 °, oil absorption is 14.6g/g.
Embodiment 3
(1) weigh 0.395g particles of polylactic acid respectively with me104e prunus mume (sieb.) sieb.et zucc. Teller-Tuo Li electronic balance, be dissolved in 2ml dichloro
In methane, at ambient temperature, it is allowed to be stirred well to and is completely dissolved, obtain the PLA solution that concentration is 13%.
(2) by the PLA solution having configured, under the stirring of magnetic stirring apparatuss, add the kapok that 0.07g length is 5mm
Fiber, stirs, and dropwise to solution to being separated, room temperature stands 24h to Deca 3ml poor solvent, takes out, is immersed in no water beetle
In alcohol, it is placed in vibration on shaking table, after changing repeatedly, is vacuum dried under room temperature, obtain polylactic acid/kapok long fibre compound many
Porous materials.
(3) test the oil absorbency of this composite porous material, the porosity of this porous material is 87.3%, and water contact angle is
139.8 °, oil absorption is 18g/g.
Embodiment 4
(1) weigh 0.395g particles of polylactic acid respectively with me104e prunus mume (sieb.) sieb.et zucc. Teller-Tuo Li electronic balance, be dissolved in 2ml dichloro
In methane, at ambient temperature, it is allowed to be stirred well to and is completely dissolved, obtain the PLA solution that concentration is 13%.
(2) by the PLA solution having configured, under the stirring of magnetic stirring apparatuss, add the cattle that 0.07g length is 0.2mm
JIAOGUA fiber, stirs, and dropwise to solution to being separated, room temperature stands 24h to Deca 3ml poor solvent, takes out, and is immersed in no
In water methanol, it is placed in vibration on shaking table, after changing repeatedly, be vacuum dried under room temperature, obtain polylactic acid/Radix Calotropis giganteae chopped fiber
Composite porous material.
(3) test the oil absorbency of this composite porous material, the porosity of this porous material is 85%, and water contact angle is
130 °, oil absorption is 15.8g/g.
Claims (10)
1. a kind of preparation method of three-dimensional porous oil absorption material, comprising:
(1) polylactic acid is dissolved in a solvent, stirring and dissolving, obtain PLA solution；
(2), under stirring condition, become cloudy being added dropwise over poor solvent in the PLA solution of step (1) by clarification to solution,
Room temperature stands, displacement, and vacuum drying obtains three-dimensional porous oil absorption material；
Or under agitation, natural fiber will be added in the PLA solution of step (1), be then added dropwise over poor solvent extremely
Solution is separated, and room temperature stands, and displacement obtains final product three-dimensional porous oil absorption material.
2. a kind of three-dimensional porous oil absorption material according to claim 1 preparation method it is characterised in that: described step
(1) molecular weight 6.0 × 10 of polylactic acid in4～1.0 × 105g/mol；Solvent is dichloromethane.
3. a kind of three-dimensional porous oil absorption material according to claim 1 preparation method it is characterised in that: described step
(1) in, the mass percentage concentration of PLA solution is 10%～20%.
4. a kind of three-dimensional porous oil absorption material according to claim 1 preparation method it is characterised in that: described step
(2) in, poor solvent is one or more of acetone, dehydrated alcohol, absolute methanol, normal hexane, hexamethylene.
5. a kind of three-dimensional porous oil absorption material according to claim 1 preparation method it is characterised in that: in step (1)
Solvent and step (2) in poor solvent volume ratio be 1:0.5～1:1.5.
6. a kind of three-dimensional porous oil absorption material according to claim 1 preparation method it is characterised in that: described step
(2) in, natural fiber is one or more of bombax cotton, Radix Calotropis giganteae fibre.
7. a kind of three-dimensional porous oil absorption material according to claim 1 preparation method it is characterised in that: in step (2)
In natural fiber and polylactic acid blend system, natural fiber is 1:10～1:2 with the mass ratio of polylactic acid.
8. a kind of three-dimensional porous oil absorption material according to claim 1 preparation method it is characterised in that: described step
(2) in, the length of natural fiber is 0.2mm～5mm.
9. a kind of three-dimensional porous oil absorption material according to claim 1 preparation method it is characterised in that: described step
(2) in, room temperature time of repose is 10-24h.
10. a kind of three-dimensional porous oil absorption material according to claim 1 preparation method it is characterised in that: described step
(2) it is replaced into methanol replacement in, particularly as follows: being immersed in absolute methanol, being placed in vibration on shaking table, changing 1-5 time.
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| CN201611007945.1A CN106334543A (en) | 2016-11-16 | 2016-11-16 | Method for preparing three-dimensional porous oil absorption material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107082855A (en) * | 2017-06-01 | 2017-08-22 | 合肥创沃科技有限公司 | A kind of PLA is combined the preparation method of kapok fiber oil absorption material |
| CN107653684A (en) * | 2017-09-30 | 2018-02-02 | 兰州大学 | A kind of polysulfones/natural fiber compound oil absorption material and preparation method thereof |
| CN108221384A (en) * | 2017-12-29 | 2018-06-29 | 广东工业大学 | A kind of preparation method of acid fiber by polylactic composite surface porous film material |
| CN110218423A (en) * | 2019-06-03 | 2019-09-10 | 东华镜月（苏州）纺织技术研究有限公司 | A kind of three-dimensional porous compound Monolithic Columns of polylactic acid and caprolactone and preparation method thereof |
| WO2020238270A1 (en) * | 2019-05-29 | 2020-12-03 | 南京大学 | Modified polylactic acid non-woven fabric for oil-water separation, preparation method therefor and application thereof |
| CN112725906A (en) * | 2020-12-29 | 2021-04-30 | 河北工业大学 | Electrostatic spinning preparation method of porous polylactic acid fiber oil absorption material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107082855A (en) * | 2017-06-01 | 2017-08-22 | 合肥创沃科技有限公司 | A kind of PLA is combined the preparation method of kapok fiber oil absorption material |
| CN107653684A (en) * | 2017-09-30 | 2018-02-02 | 兰州大学 | A kind of polysulfones/natural fiber compound oil absorption material and preparation method thereof |
| CN108221384A (en) * | 2017-12-29 | 2018-06-29 | 广东工业大学 | A kind of preparation method of acid fiber by polylactic composite surface porous film material |
| CN108221384B (en) * | 2017-12-29 | 2021-03-16 | 广东工业大学 | Preparation method of polylactic acid fiber composite surface porous membrane material |
| WO2020238270A1 (en) * | 2019-05-29 | 2020-12-03 | 南京大学 | Modified polylactic acid non-woven fabric for oil-water separation, preparation method therefor and application thereof |
| GB2598511A (en) * | 2019-05-29 | 2022-03-02 | Nanjing University | Modified polylactic acid non-woven fabric for oil-water separation, preparation method therefor and application thereof |
| GB2598511B (en) * | 2019-05-29 | 2022-07-06 | Nanjing University | Modified polylactic acid nonwoven fabric for oil/water separation and preparation method and application thereof |
| CN110218423A (en) * | 2019-06-03 | 2019-09-10 | 东华镜月（苏州）纺织技术研究有限公司 | A kind of three-dimensional porous compound Monolithic Columns of polylactic acid and caprolactone and preparation method thereof |
| CN112725906A (en) * | 2020-12-29 | 2021-04-30 | 河北工业大学 | Electrostatic spinning preparation method of porous polylactic acid fiber oil absorption material |
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Application publication date: 20170118 |