CN112973474A - Preparation of silicon carbide micro-filtration membrane - Google Patents
Preparation of silicon carbide micro-filtration membrane Download PDFInfo
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- CN112973474A CN112973474A CN201911210356.7A CN201911210356A CN112973474A CN 112973474 A CN112973474 A CN 112973474A CN 201911210356 A CN201911210356 A CN 201911210356A CN 112973474 A CN112973474 A CN 112973474A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/147—Microfiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/38—Hydrophobic membranes
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a preparation method of a silicon carbide micro-filtration membrane, wherein the hydrophobic modification of the SiC micro-filtration membrane is realized by respectively taking n-octyl triethoxysilane and ethanol as a modifier and a solvent and grafting a hydrophobic layer by a graft polymerization method. The modified hydrophobic ceramic membrane has good hydrophobic effect, the oil-solid separation operation is continuously operated for 36 hours, and the hydrophobic ceramic membrane has good stability.
Description
Technical Field
The present invention relates to the field of film preparation.
Background
With the development of industrialization, a large amount of waste oil is generated in the industries of petrochemical industry, mechanical manufacturing, food and medicine and the like. It is reported that about 32 million tons of waste oil are discharged into water every year, causing environmental pollution and waste of resources. Therefore, oil-containing system separation is receiving increasing attention. Depending on the continuous and dispersed phases, researchers have generally divided oil-containing systems into three categories: oily wastewater, aqueous oil and solid oil. The main phase in the oily wastewater is water, and the hydrophilic membrane is selected to carry out effective separation, so that the method is widely applied to the fields of oilfield produced water and the like. The separation difficulty of the aqueous oil liquid and the solid oil liquid is high because the main phase of the aqueous oil liquid and the solid oil liquid is oil, and the research of the separation of the oil-containing system is mainly focused on the two types at present. The existing separation method such as the gravity settling method is simple to operate, but has long time consumption and low efficiency; the chemical demulsification method has good separation effect, but is easy to produce secondary pollution. The hydrophobic-oleophilic membrane material developed in recent years has higher wettability to oil and can prevent water drops from permeating, and can effectively reduce membrane pollution and improve membrane flux in the separation of an oil-containing system with oil as a main phase. Because most of organic membranes are hydrophobic membranes and are low in price, researchers mostly adopt the organic hydrophobic membranes to carry out experimental research in the early period. But the organic membrane is easy to swell when being contacted with organic solvents such as oil for a long time, and the service life of the membrane is influenced; and the organic film is not resistant to high temperature and is not suitable for oil product separation at high temperature. The ceramic membrane has the characteristics of good chemical stability, high temperature resistance, long service life and the like, and has unique advantages in the separation of an oil-containing system.
Disclosure of Invention
The invention aims to provide a method for hydrophobically modifying a silicon carbide film.
The technical scheme of the invention is as follows:
a hydrophobic modification method for a silicon carbide film is characterized in that the hydrophobic modification of a SiC microfiltration membrane takes n-octyl triethoxysilane and ethanol as a modifier and a solvent respectively, a graft polymerization method is adopted, and the hydrophobic modification of a ceramic membrane mainly comprises two steps: firstly, a hydrolyzable group of organosilane is hydrolyzed in a solvent, and the hydrolyzable group is hydrolyzed into silanol; then, silanol and hydroxyl (-OH) on the surface of the ceramic membrane undergo dehydration condensation reaction, so that organosilane is grafted on the surface of the SiC membrane in a covalent bond Si-O-Si mode. Boiling the blank SiC microfiltration membrane in boiling water for 3 h, and drying at 100 ℃ for 12 h for later use. Then dissolving n-octyl triethoxysilane in anhydrous ethanol to prepare a solution with a concentration of 0.05-0.5 mol.L−1The modified liquid of (1). Then the pretreated ceramic membrane is put into a beaker filled with a modified solution and is placed on a magnetic stirrer, and the stirring speed is fixed at 300 r.min−1Heating the modified solutionTo 20-60 ℃. After reacting for 4-24 h, washing the ceramic membrane for 10 min by using ethanol, ethanol and deionized water mixed liquor (volume ratio = 1: 1) and deionized water respectively in sequence. And finally, drying the ceramic membrane in an oven at 85 ℃ for 5 hours to obtain the hydrophobic SiC membrane.
Oil solid separation experiment 2060 g of 260#Mixing solvent oil with 2.06 g of pigment carbon black with average particle diameter of 2.4 μm at 700 r min−1Stirring for 12 hours at the rotating speed of (2.5L) to prepare an oil-solid mixed solution with the solid content of 0.1%. And (3) carrying out an oil-solid separation experiment by adopting a ceramic membrane cross-flow filtering device. The oil-solid mixed liquid in the raw material tank is driven to the membrane component by a pump, and the penetrating fluid permeates the separation membrane under the pushing of the pressure difference. The permeation flux measured 30 min after the filtration process had stabilized was taken as the steady-state flux. The experimental process adopts a full reflux mode. During backflushing, compressed air is used to push the penetrating fluid in the backflushing tank to reversely permeate the membrane layer, and the volume of the penetrating fluid backflushing each time is 150 ml. Controlling the back flushing pressure to be 0.5 MPa, the back flushing time to be 3 s and the back flushing period to be 30 min.
Has the advantages that: the SiC membrane is good in hydrophobic effect after being modified, the oil-solid separation operation is continuously operated for 36 hours, and the hydrophobic ceramic membrane has good stability.
Detailed Description
Firstly, a hydrolyzable group of organosilane is hydrolyzed in a solvent, and the hydrolyzable group is hydrolyzed into silanol; then, silanol and hydroxyl (-OH) on the surface of the ceramic membrane undergo dehydration condensation reaction, so that organosilane is grafted on the surface of the SiC membrane in a covalent bond Si-O-Si mode. Boiling the blank SiC microfiltration membrane in boiling water for 3 h, and drying at 100 ℃ for 12 h for later use. Then dissolving n-octyl triethoxysilane in anhydrous ethanol to prepare a solution with a concentration of 0.05-0.5 mol.L−1The modified liquid of (1). Then the pretreated ceramic membrane is put into a beaker filled with a modified solution and is placed on a magnetic stirrer, and the stirring speed is fixed at 300 r.min−1Heating the modified liquid to 20-60 ℃. After reacting for 4-24 h, washing the ceramic membrane for 10 min by using ethanol, ethanol and deionized water mixed liquor (volume ratio = 1: 1) and deionized water respectively in sequence. And finally, drying the ceramic membrane in an oven at 85 ℃ for 5 hours to obtain the hydrophobic SiC membrane.
The steady-state flux 1316 Lm of the hydrophobic SiC membrane is under the transmembrane pressure difference of 0.2 MPa−2·h−1. The oil-solid separation operation is continuously operated for 36 hours, which shows that the hydrophobic ceramic membrane has better stability.
Claims (1)
1. A method for hydrophobic modification of a silicon carbide film is characterized in that the hydrophobic modification of the SiC microfiltration membrane takes n-octyl triethoxysilane and ethanol as a modifier and a solvent respectively:
firstly, a hydrolyzable group of organosilane is hydrolyzed in a solvent, and the hydrolyzable group is hydrolyzed into silanol; then, carrying out dehydration condensation reaction on silanol and hydroxyl on the surface of the ceramic membrane so as to graft organosilane on the surface of the SiC membrane in a covalent bond Si-O-Si manner; boiling the blank SiC microfiltration membrane in boiling water for 3 h, and drying at 100 ℃ for 12 h for later use;
then dissolving n-octyl triethoxysilane in anhydrous ethanol to prepare a solution with a concentration of 0.05-0.5 mol.L−1The modifying solution of (4);
then the pretreated ceramic membrane is put into the modifying solution and placed on a magnetic stirrer, and the stirring speed is fixed at 300 r.min−1Heating the modified solution to 20-60 ℃ and reacting for 4-24 h;
sequentially washing the ceramic membrane for 10 min by using ethanol, ethanol and deionized water mixed solution (volume ratio = 1: 1) and deionized water respectively; and finally, drying the ceramic membrane in an oven at 85 ℃ for 5 hours to obtain the hydrophobic SiC membrane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911210356.7A CN112973474A (en) | 2019-12-02 | 2019-12-02 | Preparation of silicon carbide micro-filtration membrane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911210356.7A CN112973474A (en) | 2019-12-02 | 2019-12-02 | Preparation of silicon carbide micro-filtration membrane |
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| Publication Number | Publication Date |
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| CN112973474A true CN112973474A (en) | 2021-06-18 |
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| CN201911210356.7A Pending CN112973474A (en) | 2019-12-02 | 2019-12-02 | Preparation of silicon carbide micro-filtration membrane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114685188A (en) * | 2022-03-18 | 2022-07-01 | 宁夏大学 | Super-hydrophobic silicon carbide ceramic membrane and preparation method thereof |
-
2019
- 2019-12-02 CN CN201911210356.7A patent/CN112973474A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 李秀秀等: "Al2O3和SiC 微滤膜的疏水改性及其油固分离性能研究", 《化工学报》, vol. 70, no. 7, pages 2737 - 2747 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114685188A (en) * | 2022-03-18 | 2022-07-01 | 宁夏大学 | Super-hydrophobic silicon carbide ceramic membrane and preparation method thereof |
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