CN108097055B - Coating method of hollow fiber membrane for oil gas recovery - Google Patents
Coating method of hollow fiber membrane for oil gas recovery Download PDFInfo
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- CN108097055B CN108097055B CN201711311999.1A CN201711311999A CN108097055B CN 108097055 B CN108097055 B CN 108097055B CN 201711311999 A CN201711311999 A CN 201711311999A CN 108097055 B CN108097055 B CN 108097055B
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Abstract
The invention relates to the technical field of separation membranes, in particular to a coating method of a hollow fiber membrane for oil gas recovery. The coating method of the hollow fiber membrane adopts glow discharge low-temperature plasma polymerization to coat the polyvinylidene fluoride hollow fiber membrane base membrane, the method is convenient and fast, the operation is simple, the coating thickness of the obtained hollow fiber membrane is thin, and the oil gas recovery efficiency is high and can reach more than 97%.
Description
Technical Field
The invention relates to the technical field of separation membranes, in particular to a plating method of a hollow fiber membrane for oil gas recovery.
Background
The oil gas recovery means that volatile gasoline oil gas is collected in the processes of loading and unloading gasoline and refueling a vehicle, so that the atmospheric pollution caused by the volatilization of the oil gas is prevented, and potential safety hazards are eliminated. The common methods at present include absorption method, condensation method, membrane separation method, adsorption method and the like. The membrane separation method utilizes the characteristic that a special polymer membrane has preferential permeability to hydrocarbons, so that oil gas molecules preferentially permeate the polymer membrane and air components are trapped and discharged, the removal efficiency is high, and the membrane separation method is energy-saving and environment-friendly. The polymeric membrane used for oil-gas separation can be divided into a homogeneous membrane, an asymmetric membrane and a composite membrane according to the structure. The composite membrane is prepared by firstly preparing a porous supporting layer and then covering an ultrathin compact skin layer on the surface of the porous supporting layer, wherein the ultrathin compact skin layer plays a role in separating gas and is also called as a functional layer. According to the mechanism of separating gas by the functional layer, the thinner the functional layer is, the larger the gas film flux is. The optimal thickness of the functional layer is 0.5-1 mu m, but the coating technology of the current separation layer is not perfect, the most common method is an immersion pulling method, and the thickness of the functional layer of the flat membrane prepared by the method is about several microns. The hollow fiber gas separation membrane is a hollow fiber membrane with the function of separating mixed gas, and has a structure which is more special than that of a flat membrane, so that the coating of the hollow fiber membrane is more difficult, the thickness of the coating is larger than that of the flat membrane, and the oil gas recovery efficiency is low.
Disclosure of Invention
Aiming at the problem of low oil gas recovery efficiency caused by the fact that the existing hollow fiber membrane is thick, the invention aims to provide a coating method of the hollow fiber membrane for oil gas recovery, which can obtain the hollow fiber membrane with a thin coating layer, and has high oil gas recovery efficiency, and the preparation method is convenient and easy to operate.
The invention provides the following technical scheme:
a hollow fiber membrane plating method for oil gas recovery, placing a hollow fiber membrane base membrane in a plating device in an argon and air mixed atmosphere, plating a monomer solution on the hollow fiber membrane base membrane through glow discharge low-temperature plasma polymerization, wherein the plating device comprises an air inlet pipe, a liquid inlet pipe and a glow discharge pipe which are horizontally connected in sequence:
the port of the air inlet pipe, which is far away from the liquid inlet pipe, is provided with a vacuum valve, a vacuum pump communicated with the air inlet pipe is arranged close to the vacuum valve, the side surface of the air inlet pipe is provided with three openings, two of the openings are connected with an air inlet valve, and the rest of the openings are connected with a vacuum gauge;
the liquid inlet pipe is a T-shaped pipe, two ends of a horizontal section of the liquid inlet pipe are respectively connected with the gas inlet pipe and the glow discharge tube, a free port extending downwards from the vertical section is communicated with a monomer liquid pool containing monomer solution, two needle valves are arranged in the horizontal section and are arranged on two sides of the vertical section, the needle valves are also arranged in the vertical section, and the monomer liquid pool is arranged in the water bath pool;
the outer side of the glow discharge tube is wound with a plurality of coils, and the coils are connected with a radio frequency power generator.
As an improvement of the method of the invention, the plating method comprises the following steps:
(1) soaking the hollow fiber membrane base membrane in isopropanol for 2-3 hours, taking out, vacuum-drying for 10-20 minutes, and then vacuumizing;
(2) placing the hollow fiber membrane basal membrane in a glow discharge tube, and sealing the glow discharge tube at two ends of the hollow fiber membrane by silicon rubber plugs;
(3) adding the monomer solution into the monomer solution pool, adding water into the water bath pool to keep the water bath constant;
(4) opening two needle valves at the horizontal section in the liquid inlet pipe under the closing state of a vacuum valve, introducing argon and air into the air inlet pipe through an air inlet valve, opening a vacuum pump to keep the pressure in the coating device to be 0.65-2.00 Pa, and starting a radio frequency power generator to perform glow discharge;
(5) opening a needle valve of a vertical section of the liquid inlet pipe under the glow discharge condition, keeping the pressure in the plating device for 25-30 seconds after the pressure reaches 26.6Pa, and then closing the needle valve of the vertical section;
(6) and closing the radio frequency power generator, stopping introducing the argon and the air, and taking out the hollow fiber membrane at room temperature.
As an improvement of the method, the hollow fiber membrane base membrane is polyvinylidene fluoride hollow fiber membrane base membrane.
As a modification of the process of the invention, the monomer solution is an aqueous hexamethyldisiloxane solution having a mass concentration of 98%.
As an improvement of the method of the invention, the step (3) is as follows: adding a hexamethyldisiloxane aqueous solution into a monomer liquid pool, closing a vacuum valve, opening a needle valve in a liquid inlet pipe, adding ice blocks into a water bath pool, vacuumizing for 10-15 minutes until the pressure in a plating device is 0.65-2.00 Pa, then closing a vacuum pump for 10-15 minutes, then opening the vacuum pump again, repeating the vacuumizing for 3 times, closing the needle valve in the liquid inlet pipe, and adding water into the water bath pool to keep the water bath constant temperature at 70-73 ℃.
As an improvement of the method, the volume ratio of the argon to the nitrogen in the step (4) is 1:1, the frequency of a radio frequency power supply of the radio frequency power generator is 13.56MHz, and the power is 800-1000W.
As an improvement of the method according to the invention, the glow discharge vessel is cylindrical.
The coating method of the hollow fiber membrane adopts glow discharge low-temperature plasma polymerization to coat the hollow fiber membrane substrate, the polyvinylidene fluoride hollow fiber membrane substrate is placed in a glow discharge tube, an electric field with the frequency of 13.56MHz and the power of 800-1000W is applied to mixed gas of argon and air in the volume ratio of 1:1 under the condition of low pressure of 0.65-2 Pa to carry out glow discharge, and a small amount of free electrons in the mixed gas are accelerated along the direction of the electric field. Due to the low pressure and long distance, the movement of the free electrons tends to extremely high speed and thus obtains extremely large kinetic energy. When the high-energy electrons collide with molecules or atoms of monomer gas evaporated from the monomer solution, the molecules or atoms are excited, dissociated or broken to form various excited molecules, atoms, free radicals and electrons, the whole monomer gas is in an ionized state, the gas is wrapped by a hollow fiber membrane after being dissociated, a separation layer is formed after cooling, and the selected hexamethyldisiloxane monomer is nonflammable, belongs to a semi-inorganic and semi-organic structure and has good gas permeability. The method is simple, the coating efficiency is high, and the coating thickness is thin.
The invention has the following beneficial effects:
the coating method of the hollow fiber membrane adopts glow discharge low-temperature plasma polymerization to coat the polyvinylidene fluoride hollow fiber membrane base membrane, the method is convenient and fast, the operation is simple, the coating thickness of the obtained hollow fiber membrane is thinner, and the oil gas recovery efficiency is high.
Drawings
FIG. 1 shows a coating apparatus used in the method of the present invention.
Fig. 2 is a structural diagram of a light discharge tube.
In the figure: 1. the device comprises an air inlet pipe, 11, a vacuum valve, 12, a vacuum pump, 13, an air inlet valve, 14, a vacuum gauge, 2, a liquid inlet pipe, 21, a needle valve, 22, a monomer liquid pool, 3, a glow discharge tube, 31, a silicon rubber plug, 4, a radio frequency power generator, 41, a coil, 5, a water bath pool, 6 and a hollow fiber membrane base membrane.
Detailed Description
The following further describes the embodiments of the present invention.
The starting materials used in the present invention are commercially available or commonly used in the art, unless otherwise specified, and the methods in the following examples are conventional in the art, unless otherwise specified.
The coating conversion device used in the method disclosed by the invention is shown in figures 1-2 and comprises an air inlet pipe 1, a liquid inlet pipe 2 and a glow discharge tube 3 which are horizontally connected in sequence, wherein a vacuum valve 11 is arranged at a port of the air inlet pipe, which is far away from the liquid inlet pipe, a vacuum pump 12 communicated with the air inlet pipe is arranged close to the vacuum valve, three openings are arranged on the side surface of the air inlet pipe, two of the openings are connected with an air inlet valve 13, and the rest of the openings are connected with a; the liquid inlet pipe is a T-shaped pipe, two ends of a horizontal section of the liquid inlet pipe are respectively connected with the gas inlet pipe and the glow discharge tube, a free port extending downwards of the vertical section is communicated with a monomer liquid pool 22 containing monomer solution, two needle valves 21 are arranged in the horizontal section and are arranged on two sides of the vertical section, the needle valves are also arranged in the vertical section, and the monomer liquid pool is arranged in the water bath pool 5; the glow discharge is cylindrical and is wound with a number of turns 41 on the outside, the turns being connected to a radio frequency power generator 4.
Example 1
A hollow fiber membrane plating method for oil gas recovery, the hollow fiber membrane basement membrane 6 is placed in a plating device with argon and air mixed atmosphere, monomer solution is plated on the hollow fiber membrane basement membrane through glow discharge low-temperature plasma polymerization, the hollow fiber membrane basement membrane is polyvinylidene fluoride hollow fiber membrane basement membrane, the monomer solution is hexamethyldisiloxane water solution with mass concentration of 98%, and the method comprises the following steps:
(1) soaking a polyvinylidene fluoride hollow fiber membrane base membrane in isopropanol for 2 hours, taking out the polyvinylidene fluoride hollow fiber membrane base membrane, performing vacuum drying in a vacuum drying oven for 10 minutes, and then placing the polyvinylidene fluoride hollow fiber membrane base membrane in the vacuum oven for vacuumizing;
(2) placing the treated polyvinylidene fluoride hollow fiber membrane substrate membrane in a cylindrical glow discharge tube, and sealing the glow discharge tube at two ends of the hollow fiber membrane by silicon rubber plugs 31;
(3) adding hexamethyldisiloxane aqueous solution into the monomer liquid pool, closing a vacuum valve, opening a needle valve in a liquid inlet pipe, adding ice blocks into the water bath pool, vacuumizing for 10 minutes until the pressure in the plating device is 0.65Pa, then closing the vacuum valve for 10 minutes, then opening again, repeating the vacuumizing for 3 times, closing the needle valve in the liquid inlet pipe, adding water into the water bath pool, and keeping the water bath constant temperature at 70 ℃;
(4) opening two needle valves at the horizontal section in the liquid inlet pipe under the closing state of a vacuum valve, introducing argon and air into the gas inlet pipe through the gas inlet valve respectively, wherein the volume ratio of the argon to the air is 1:1, opening a vacuum pump to keep the pressure in the coating device to be 0.65Pa, and starting a radio frequency power generator to perform glow discharge, wherein the frequency of a radio frequency power supply is 13.56MHz, and the power is 800W;
(5) opening a needle valve of a vertical section of the liquid inlet pipe under the condition of glow discharge, allowing monomer gas evaporated from the monomer solution to enter the glow discharge pipe to increase the pressure in the plating device to 26.6Pa, keeping the pressure for 25 seconds, and then closing the needle valve of the vertical section;
(6) and closing the radio frequency power generator, stopping introducing the argon and the air, and taking out the hollow fiber membrane at room temperature.
Example 2
A hollow fiber membrane plating method for oil gas recovery, the hollow fiber membrane basement membrane 6 is placed in a plating device with argon and air mixed atmosphere, monomer solution is plated on the hollow fiber membrane basement membrane through glow discharge low-temperature plasma polymerization, the hollow fiber membrane basement membrane is polyvinylidene fluoride hollow fiber membrane basement membrane, the monomer solution is hexamethyldisiloxane water solution with mass concentration of 98%, and the method comprises the following steps:
(1) soaking a polyvinylidene fluoride hollow fiber membrane base membrane in isopropanol for 2.5 hours, taking out the polyvinylidene fluoride hollow fiber membrane base membrane, performing vacuum drying in a vacuum drying oven for 15 minutes, and then placing the polyvinylidene fluoride hollow fiber membrane base membrane in the vacuum oven for vacuumizing;
(2) placing the treated polyvinylidene fluoride hollow fiber membrane substrate membrane in a cylindrical glow discharge tube, and sealing the glow discharge tube at two ends of the hollow fiber membrane by silicon rubber plugs 31;
(3) adding hexamethyldisiloxane aqueous solution into the monomer liquid pool, closing a vacuum valve, opening a needle valve in a liquid inlet pipe, adding ice blocks into the water bath pool, vacuumizing after 13 minutes until the pressure in the plating device is 1.5Pa, then closing the vacuum valve for 13 minutes, then opening again, repeating the vacuumizing for 3 times, closing the needle valve in the liquid inlet pipe, adding water into the water bath pool, and keeping the water bath constant temperature at 72 ℃;
(4) opening two needle valves at the horizontal section in the liquid inlet pipe under the closing state of a vacuum valve, introducing argon and air into the gas inlet pipe through the gas inlet valve respectively, wherein the volume ratio of the argon to the air is 1:1, opening a vacuum pump to keep the pressure in the coating device to be 1.5Pa, and starting a radio frequency power generator to perform glow discharge, wherein the frequency of a radio frequency power supply is 13.56MHz, and the power is 900W;
(5) opening a needle valve of a vertical section of the liquid inlet pipe under the condition of glow discharge, allowing monomer gas evaporated from the monomer solution to enter the glow discharge pipe to increase the pressure in the plating device to 26.6Pa, keeping the pressure for 28 seconds, and then closing the needle valve of the vertical section;
(6) and closing the radio frequency power generator, stopping introducing the argon and the air, and taking out the hollow fiber membrane at room temperature.
Example 3
A hollow fiber membrane plating method for oil gas recovery, the hollow fiber membrane basement membrane 6 is placed in a plating device with argon and air mixed atmosphere, monomer solution is plated on the hollow fiber membrane basement membrane through glow discharge low-temperature plasma polymerization, the hollow fiber membrane basement membrane is polyvinylidene fluoride hollow fiber membrane basement membrane, the monomer solution is hexamethyldisiloxane water solution with mass concentration of 98%, and the method comprises the following steps:
(1) soaking a polyvinylidene fluoride hollow fiber membrane base membrane in isopropanol for 3 hours, taking out the polyvinylidene fluoride hollow fiber membrane base membrane, performing vacuum drying in a vacuum drying oven for 20 minutes, and then placing the polyvinylidene fluoride hollow fiber membrane base membrane in the vacuum oven for vacuumizing;
(2) placing the treated polyvinylidene fluoride hollow fiber membrane substrate membrane in a cylindrical glow discharge tube, and sealing the glow discharge tube at two ends of the hollow fiber membrane by silicon rubber plugs 31;
(3) adding hexamethyldisiloxane aqueous solution into the monomer liquid pool, closing a vacuum valve, opening a needle valve in a liquid inlet pipe, adding ice blocks into the water bath pool, vacuumizing for 15 minutes until the pressure in the plating device is 2.00Pa, then closing the vacuum pump for 15 minutes, then opening the vacuum pump again, repeating the vacuumizing for 3 times, closing the needle valve in the liquid inlet pipe, adding water into the water bath pool, and keeping the water bath constant temperature at 73 ℃;
(4) opening two needle valves at the horizontal section in the liquid inlet pipe under the closing state of a vacuum valve, introducing argon and air into the gas inlet pipe through the gas inlet valve respectively, wherein the volume ratio of the argon to the air is 1:1, opening a vacuum pump to keep the pressure in the coating device to be 2.00Pa, and starting a radio frequency power generator to perform glow discharge, wherein the frequency of a radio frequency power supply is 13.56MHz, and the power is 1000W;
(5) opening a needle valve of a vertical section of the liquid inlet pipe under the condition of glow discharge, allowing monomer gas evaporated from the monomer solution to enter the glow discharge pipe to increase the pressure in the plating device to 26.6Pa, keeping the pressure for 30 seconds, and then closing the needle valve of the vertical section;
(6) and closing the radio frequency power generator, stopping introducing the argon and the air, and taking out the hollow fiber membrane at room temperature.
Hollow fiber membrane oil gas recovery performance
And (3) respectively recycling the organic mixed steam VOCs raw gas to be treated through membrane components prepared by the hollow fiber membranes obtained in the embodiments 1-3 to obtain purified oil gas and concentrated oil gas, and analyzing the content of each component of the purified oil gas and the concentrated oil gas through gas chromatography. The test results are shown in table 1 below.
TABLE 1 test results
As can be seen from the above table, the hollow fiber membrane obtained by glow discharge low-temperature plasma polymerization method has good oil gas recovery effect and high oil gas recovery efficiency, and the concentration of the purified oil gas of the VOCs raw gas treated by the membrane module prepared from the hollow fiber membranes of examples 1 to 3 is respectively reduced to 4.15 × 103mg/m3、4.30×103mg/m3And 4.26X 103mg/m3And the oil gas recovery rate reaches more than 97 percent when the oil gas reaches the secondary emission standard of the atmospheric pollutant emission standard of the GB20950-2007 oil storage warehouse.
Claims (5)
1. A coating method of a hollow fiber membrane for oil gas recovery, the used coating device comprises an air inlet pipe, a liquid inlet pipe and a glow discharge pipe which are horizontally connected in sequence:
the port of the air inlet pipe, which is far away from the liquid inlet pipe, is provided with a vacuum valve, a vacuum pump communicated with the air inlet pipe is arranged close to the vacuum valve, the side surface of the air inlet pipe is provided with three openings, two of the openings are connected with an air inlet valve, and the rest of the openings are connected with a vacuum gauge;
the liquid inlet pipe is a T-shaped pipe, two ends of a horizontal section of the liquid inlet pipe are respectively connected with the gas inlet pipe and the glow discharge tube, a free port extending downwards from the vertical section is communicated with a monomer liquid pool containing monomer solution, two needle valves are arranged in the horizontal section and are arranged on two sides of the vertical section, the needle valves are also arranged in the vertical section, and the monomer liquid pool is arranged in the water bath pool;
a plurality of coils are wound on the outer side of the glow discharge tube, the coils are connected with a radio frequency power generator,
the method is characterized in that a hollow fiber membrane base membrane is placed in a coating device in a mixed atmosphere of argon and air, and a monomer solution is coated on the hollow fiber membrane base membrane through glow discharge low-temperature plasma polymerization, and the method comprises the following steps:
(1) soaking the hollow fiber membrane base membrane in isopropanol for 2-3 hours, taking out, vacuum-drying for 10-20 minutes, and then vacuumizing;
(2) the hollow fiber membrane substrate film is arranged in a glow discharge tube, and the two ends close to the hollow fiber membrane are sealed by silicon rubber plugs to the glow discharge tube;
(3) adding the monomer solution into the monomer solution pool, adding water into the water bath pool to keep the water bath constant;
(4) opening two needle valves at the horizontal section in the liquid inlet pipe under the closing state of a vacuum valve, introducing argon and air into the air inlet pipe through an air inlet valve, opening a vacuum pump to keep the pressure in the coating device to be 0.65-2.00 Pa, and starting a radio frequency power generator to perform glow discharge;
(5) opening a needle valve of a vertical section of the liquid inlet pipe under the glow discharge condition, keeping the pressure in the plating device for 25-30 seconds after the pressure reaches 26.6Pa, and then closing the needle valve of the vertical section;
(6) closing the radio frequency power generator, stopping introducing argon and air, and taking out the hollow fiber membrane at room temperature;
the volume ratio of argon to nitrogen in the step (4) is 1: 1;
the monomer solution was an aqueous hexamethyldisiloxane solution having a mass concentration of 98%.
2. The plating method according to claim 1, wherein the hollow fiber membrane-based membrane is a polyvinylidene fluoride hollow fiber membrane-based membrane.
3. The plating method according to claim 1, wherein the step (3) is performed by: adding a hexamethyldisiloxane aqueous solution into a monomer liquid pool, closing a vacuum valve, opening a needle valve in a liquid inlet pipe, adding ice blocks into a water bath pool, vacuumizing for 10-15 minutes until the pressure in a plating device is 0.65-2.00 Pa, then closing a vacuum pump for 10-15 minutes, then opening the vacuum pump again, repeating the vacuumizing for 3 times, closing the needle valve in the liquid inlet pipe, and adding water into the water bath pool to keep the water bath constant temperature at 70-73 ℃.
4. The plating method of claim 1, wherein the RF power generator in step (4) has an RF power frequency of 13.56MHz and a power of 800-1000W.
5. The coating method of claim 1, wherein the glow discharge tube is cylindrical.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011063940A1 (en) * | 2009-11-27 | 2011-06-03 | Gambro Lundia Ab | Hollow fibers with selective, plasma induced modification of lumen surface and continuous process for their production |
| CN103285751A (en) * | 2013-06-28 | 2013-09-11 | 清华大学 | PDMS (Polydimethylsiloxane)-PVDF (Polyvinylidene Fluoride) composite membrane for separating organic vapor and modification-preparation method thereof |
| CN106256417A (en) * | 2015-06-18 | 2016-12-28 | 中国石油化工股份有限公司 | A kind of preparation method of high-performance organic gas separation film |
| CN106906456A (en) * | 2017-01-23 | 2017-06-30 | 无锡荣坚五金工具有限公司 | A kind of preparation method of the controllable coating of the degree of cross linking |
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- 2017-12-11 CN CN201711311999.1A patent/CN108097055B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011063940A1 (en) * | 2009-11-27 | 2011-06-03 | Gambro Lundia Ab | Hollow fibers with selective, plasma induced modification of lumen surface and continuous process for their production |
| CN103285751A (en) * | 2013-06-28 | 2013-09-11 | 清华大学 | PDMS (Polydimethylsiloxane)-PVDF (Polyvinylidene Fluoride) composite membrane for separating organic vapor and modification-preparation method thereof |
| CN106256417A (en) * | 2015-06-18 | 2016-12-28 | 中国石油化工股份有限公司 | A kind of preparation method of high-performance organic gas separation film |
| CN106906456A (en) * | 2017-01-23 | 2017-06-30 | 无锡荣坚五金工具有限公司 | A kind of preparation method of the controllable coating of the degree of cross linking |
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