CN115066080B - Low-temperature normal-pressure plasma surface hydrophilic modification device and method based on carbon dioxide atmosphere - Google Patents
Low-temperature normal-pressure plasma surface hydrophilic modification device and method based on carbon dioxide atmosphereInfo
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- CN115066080B CN115066080B CN202210825179.9A CN202210825179A CN115066080B CN 115066080 B CN115066080 B CN 115066080B CN 202210825179 A CN202210825179 A CN 202210825179A CN 115066080 B CN115066080 B CN 115066080B
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
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Abstract
本发明公开了一种基于二氧化碳气氛的低温常压等离子体表面亲水改性装置及方法，该装置包括二氧化碳供气单元、等离子体处理室及传送带，等离子体处理室包括发生室和后置反应室，发生室内设有正电极、负电极，正电极与外置控制电源电连接，负电极接地；二氧化碳供气单元位于等离子体处理室的顶部，二氧化碳供气单元的底部连接气管，气管延伸至发生室内的底部，二氧化碳供气单元与气管的连接处设有控制开关，控制开关与压力传感器电连接，压力传感器位于发生室内的顶部；传送带为U型结构，传送带依次穿过发生室和后置反应室，正电极位于传送带的上部，负电极位于传送带的下部。该发明的装置及方法能够连续制备改性薄膜。
The present invention discloses a low-temperature, atmospheric-pressure plasma surface hydrophilic modification device and method based on a carbon dioxide atmosphere. The device comprises a carbon dioxide supply unit, a plasma treatment chamber, and a conveyor belt. The plasma treatment chamber comprises a generator chamber and a post-reaction chamber. The generator chamber is provided with a positive electrode and a negative electrode, the positive electrode being electrically connected to an external control power supply, and the negative electrode being grounded. The carbon dioxide supply unit is located at the top of the plasma treatment chamber, and its bottom is connected to a gas pipe extending to the bottom of the generator chamber. A control switch is provided at the connection between the carbon dioxide supply unit and the gas pipe, and the control switch is electrically connected to a pressure sensor located at the top of the generator chamber. The conveyor belt has a U-shaped structure and passes through the generator chamber and the post-reaction chamber in sequence. The positive electrode is located at the top of the conveyor belt, and the negative electrode is located at the bottom of the conveyor belt. The device and method of the invention can continuously prepare modified films.
Description
Technical Field
The invention relates to the technical field of green manufacturing, in particular to a low-temperature normal-pressure plasma surface hydrophilic modification device and method based on a carbon dioxide atmosphere.
Background
Global warming caused by carbon dioxide-based greenhouse gas emissions is severely threatening the survival and sustainable development of humans, and is one of the significant global challenges facing humans at present. In order to promote the development of green circulation and low carbon, china proposes to strive for realizing carbon peak before 2030 and realizing carbon neutralization before 2060. Meanwhile, the task of improving the environmental quality in the current stage of China is still serious, and the aim of carbon neutralization provides basic compliance for the promotion of environmental pollution control and greenhouse gas emission reduction. In order to achieve the aim of carbon neutralization, besides reducing fossil energy consumption, new energy is greatly developed, and the collection and utilization of discharged carbon dioxide can be started. There have been many studies focused on adsorption of carbon dioxide and energy regeneration. Among them, the study of catalytic decomposition of carbon dioxide by plasma technology has become one of the hot spots of carbon dioxide energy research, but the conversion rate of carbon monoxide or methane is not ideal at present, and the utilization rate of carbon dioxide is not high.
The plasma surface treatment technology is to excite gas molecules by certain energy to make the gas dissociated into excited states such as electrons, ions, free radicals, other metastable states and the like, collide with the surface of the material, break covalent bonds, generate free radicals and activate the surface of the material. While the activated material surface may combine with the excited gas to produce chemically reactive groups at the surface. Low temperature atmospheric pressure plasma processing techniques have been widely used in plating, coating, ink printing, etc. industries to enhance interfacial bonding.
In summary, carbon dioxide is taken as an atmosphere, and the carbon dioxide can be effectively activated and utilized by utilizing a plasma technology, and more hydrophilic groups are generated on the polymer film, so that the surface of the polymer film is hydrophilically modified, and the carbon dioxide is reused, and the emission of the carbon dioxide in the environment is reduced.
Disclosure of Invention
The invention aims to provide a low-temperature normal-pressure plasma surface hydrophilic modification device for carbon dioxide atmosphere, which ionizes carbon dioxide by utilizing high energy under normal pressure, so that continuous hydrophilic modification of the surface of a hydrophobic polymer film can be realized, reuse of carbon dioxide can be realized, and emission of carbon dioxide can be reduced.
In order to achieve the above purpose, the present invention provides the following technical solutions:
In one aspect, the invention provides a low-temperature normal-pressure plasma surface hydrophilic modification device based on carbon dioxide atmosphere, which comprises a carbon dioxide gas supply unit, a plasma treatment chamber and a conveyor belt,
The plasma treatment chamber comprises a generation chamber and a rear reaction chamber, wherein a positive electrode and a negative electrode are arranged in the generation chamber, the positive electrode is electrically connected with an external control power supply, and the negative electrode is grounded;
The carbon dioxide gas supply unit is positioned at the top of the plasma treatment chamber, the bottom of the carbon dioxide gas supply unit is connected with the gas pipe, the gas pipe extends to the bottom of the generation chamber, a control switch is arranged at the joint of the carbon dioxide gas supply unit and the gas pipe, the control switch is electrically connected with the pressure sensor, and the pressure sensor is positioned at the top of the generation chamber;
The conveyer belt is U type structure, and the conveyer belt passes in proper order and takes place room and rear-mounted reaction chamber, and the positive electrode is located the upper portion of conveyer belt, and the negative electrode is located the lower part of conveyer belt, and the conveyer belt embedding is between positive electrode and the negative electrode, and the negative electrode comprises two at least transfer rollers, and the transfer roller rotates and drives the conveyer belt motion, and the film of waiting to handle is attached to the conveyer belt surface.
Further, the lower left corner of the generation chamber and the upper right corner of the rear reaction chamber are provided with blowers.
Further, the spacing between the positive electrode and the negative electrode is 10mm to 500mm.
Further, the positive electrode is a rod-like or tubular electrode made of a highly conductive metal.
Further, the high conductivity metal is one of iron, copper and silver.
Further, the negative electrode is made of stainless steel, and an insulating coating is attached to the surface of the negative electrode.
Further, the insulating coating is made of Al 2O3 or Ca 0.8Sr0.2TiO3.
Further, the upper left corner of the generation chamber is provided with an inlet, the upper right corner of the rear reaction chamber is provided with an outlet, the conveyor belt enters the generation chamber from the inlet, leaves the rear reaction chamber from the outlet, the inlet and the outlet are both provided with sealing structures, and the sealing structures are 2 elastic silica gel sheets arranged in the same direction.
On the other hand, the invention also provides a low-temperature normal-pressure plasma surface hydrophilic modification method based on carbon dioxide atmosphere, which comprises the following steps:
s1, attaching a film to be treated on a conveyor belt;
S2, starting a control switch, and enabling carbon dioxide in the carbon dioxide gas supply unit to enter the generation chamber until the pressure sensor detects that the pressure in the generation chamber is equal to one atmosphere;
and S3, turning on a control power switch, starting discharge of the plasma generating electrode, rotating the conveying roller, driving the conveying belt to move by the conveying roller, and enabling the film to be processed attached to the surface of the conveying belt to sequentially pass through the generating chamber and the rear reaction chamber.
Further, the running power of the power supply is controlled to be 50W-50kW, and the discharge frequency of the positive electrode is controlled to be 10kHz-100MHz;
the running time of the film to be treated in the generating chamber is 3-5min, and the running time of the film to be treated in the post-reaction chamber is 1-3min.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the low-temperature normal-pressure plasma surface hydrophilic modification device based on the carbon dioxide atmosphere, secondary utilization of carbon dioxide is realized, the positive electrode, the negative electrode and the conveyor belt are arranged at the bottom of the reaction chamber, the inlet and the outlet of the conveyor belt are all arranged at the top of the treatment chamber, the carbon dioxide is high in specific gravity, air can be discharged from the top into the chamber, carbon dioxide gas is filled in the reaction chamber, and the generation atmosphere of the plasma is ensured to be carbon dioxide;
(2) Compared with a vacuum plasma treatment device, the device of the invention can be carried out under normal pressure without vacuum treatment, and elastic silica gel sheets arranged at the inlet and outlet positions in one way can ensure the air tightness of a treatment chamber and the continuity of input and output of a conveyor belt and realize continuous film hydrophilic treatment;
(3) According to the low-temperature normal-pressure plasma surface hydrophilic modification device based on the carbon dioxide atmosphere, plasma is used for exciting carbon dioxide ionized gas ions to bombard the surface of the film to be treated, so that the surface of the film is activated. The speed of the conveyor belt is controlled, so that the film to be treated is subjected to plasma treatment in the reaction chamber for 3-5min and then is operated in the post-reaction chamber for 1min, and the sufficient bonding reaction between the activated groups on the surface of the film and ionized gas ions is ensured. Based on experiments, the surface after plasma activation is deactivated after 1-2min in air.
(4) According to the low-temperature normal-pressure plasma surface hydrophilic modification device based on the carbon dioxide atmosphere, in the pp spunbonded non-woven fabric as an example, the contact angle of the surface of the film to water can be reduced from 95 o to 32 o, so that the hydrophilic modification of the film is successfully realized. The infrared spectrometer is used for analyzing the functional groups on the surface of the film, and the absorption peaks of hydrophilic groups-OH and C-O appear on the surface of the modified PP spun-bonded non-woven fabric.
Drawings
FIG. 1 is a schematic structural diagram of a low-temperature normal-pressure plasma surface hydrophilic modification device based on a carbon dioxide atmosphere.
1-Carbon dioxide gas supply unit, 11-gas pipe, 12-control switch, 13-pressure sensor, 2-plasma treatment chamber, 21-generation chamber, 22-post reaction chamber, 23-positive electrode, 24-negative electrode, 25-blower, 26-inlet, 27-outlet and 3-conveyor belt.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be noted that, directions or positional relationships indicated by terms such as "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", "front", "rear", etc., are directions or positional relationships based on the drawings, are merely for convenience of describing the present invention and simplifying the description, and are not to indicate or imply that the apparatus or element to be referred to must have a specific direction, be configured and operated in the specific direction, and thus should not be construed as limiting the present invention, and it should be noted that the terms "mounted", "connected" should be construed broadly, for example, may be fixedly connected, may be detachably connected, may be mechanically connected, may be indirectly connected through intermediate media, or may be electrically connected, and may be construed in a specific meaning of terms in the present invention in a specific case.
Example 1
The invention provides a low-temperature normal-pressure plasma surface hydrophilic modification device based on a carbon dioxide atmosphere, which comprises a carbon dioxide gas supply unit 1, a plasma treatment chamber 2 and a conveyor belt 3 as shown in figure 1.
The plasma processing chamber 2 comprises a generating chamber 21 and a post-reaction chamber 22, wherein a positive electrode 23 and a negative electrode 24 are arranged in the generating chamber 21, the positive electrode 23 is electrically connected with an external control power supply, and the negative electrode 24 is grounded.
The carbon dioxide gas supply unit 1 is located the top of plasma treatment room 2, and the trachea 11 is connected to the bottom of carbon dioxide gas supply unit 1, and trachea 11 extend to the bottom in the room 21, and the junction of carbon dioxide gas supply unit 1 and trachea 11 is equipped with control switch 12, and control switch is connected with pressure sensor 13 electricity, and pressure sensor 13 is located the top in the room 21.
The conveyer belt 3 is U type structure, and conveyer belt 3 passes in proper order and takes place room 21 and post-reaction chamber 22, and positive electrode 23 is located the upper portion of conveyer belt 3, and negative electrode 24 is located the lower part of conveyer belt 3, and conveyer belt 3 embeds between positive electrode 23 and the negative electrode 24, and negative electrode 24 comprises two at least transfer rollers, and the transfer roller rotates and drives conveyer belt 3 motion, and the film that waits to handle is attached to conveyer belt 3 surface.
Specifically, the carbon dioxide gas supply unit 1 can continuously supply gas to the plasma generating chamber 21, so as to ensure that the gas pressure of the generating chamber 21 is the same as the external gas pressure.
The pressure sensor 13 senses the gas pressure in the plasma processing chamber 2, and once the chamber is lower than one atmosphere, the gas is discharged through the gas pipe 11 into the bottom of the plasma processing chamber 2, so that carbon dioxide is ensured to be filled from the bottom of the generating chamber 21.
The control switch 12 includes a manual switch for exhausting air in the plasma processing chamber before plasma discharge and an automatic switch for automatically charging carbon dioxide during plasma processing.
Specifically, the lower left corner of the generation chamber 21 and the upper right corner of the post-reaction chamber 22 are provided with blowers 25. The blower 25 ensures that the ionized carbon dioxide gas fills the entire plasma processing chamber.
Specifically, the distance between the positive electrode 23 and the negative electrode 24 is 10mm to 500mm.
Specifically, the positive electrode 23 is a rod-like or tubular electrode made of a highly conductive metal.
Specifically, the high-conductivity metal is one of iron, copper and silver.
Specifically, the negative electrode 24 is made of stainless steel, and an insulating coating is attached to the surface of the negative electrode 24.
Specifically, the material of the insulating coating is Al 2O3 or Ca 0.8Sr0.2TiO3.
Specifically, the upper left corner of the generation chamber 21 is provided with an inlet 26, the upper right corner of the rear reaction chamber 22 is provided with an outlet 27, the conveyor belt 3 enters the generation chamber 21 from the inlet 26, leaves the rear reaction chamber 22 from the outlet 27, the inlet 26 and the outlet 27 are both provided with sealing structures, and the sealing structures are 2 elastic silica gel sheets arranged in the same direction. The elastic silica gel sheet is unidirectionally arranged, so that the sealing device is arranged, and meanwhile, the unidirectional operation of the conveyor belt 3 is ensured.
The device can be used for recycling carbon dioxide, and can also be used for hydrophilic modification of surfaces of coatings such as polypropylene, polyester, and the like, films, non-woven fabrics, and the like.
The contact angle of the surface of the polypropylene non-woven fabric film treated by the device of the invention to water can be reduced from 95 o to 60 o, and the hydrophilic modification of the polypropylene non-woven fabric film is successfully realized. The modified polypropylene non-woven fabric has absorption peaks of hydrophilic groups-OH and C-O.
Example 2
The invention provides a low-temperature normal-pressure plasma surface hydrophilic modification method based on a carbon dioxide atmosphere, which adopts the device and comprises the following steps:
S1, attaching a film to be treated on a conveyor belt 3;
S2, starting a control switch, and enabling carbon dioxide in the carbon dioxide gas supply unit 1 to enter the generation chamber 21 until the pressure sensor 13 detects that the pressure of the generation chamber 21 is equal to one atmosphere;
and S3, turning on a control power switch, starting discharge of the plasma generating electrode, rotating the conveying roller, driving the conveying belt 3 to move by the conveying roller, and enabling the film to be processed attached to the surface of the conveying belt 3 to sequentially pass through the generating chamber 21 and the rear reaction chamber 22.
Specifically, the operating power of the control power supply is 50W-50kW, and the discharge frequency of the positive electrode 23 is 10kHz-100MHz.
The film to be treated is run for 3-5min in the generating chamber 21 and 1-3min in the post-reaction chamber 22.
Specifically, the switch of the carbon dioxide gas supply unit 1 is manually turned on, carbon dioxide gas is charged into the bottom of the plasma processing chamber, and air is discharged from the top outlet position by using the principle that carbon dioxide is heavier than air. After 15min of inflation, the switch of the carbon dioxide gas storage tank is turned on to an automatic state, and the air blowers at the two sides of the treatment chamber are turned on, so that the gas circularly flows in the treatment chamber.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the low-temperature normal-pressure plasma surface hydrophilic modification device based on the carbon dioxide atmosphere, secondary utilization of carbon dioxide is realized, the positive electrode, the negative electrode and the conveyor belt are arranged at the bottom of the reaction chamber, the inlet and the outlet of the conveyor belt are all arranged at the top of the treatment chamber, the carbon dioxide is high in specific gravity, air can be discharged from the top into the chamber, carbon dioxide gas is filled in the reaction chamber, and the generation atmosphere of the plasma is ensured to be carbon dioxide;
(2) Compared with a vacuum plasma treatment device, the device of the invention can be carried out under normal pressure without vacuum treatment, and elastic silica gel sheets arranged at the inlet and outlet positions in one way can ensure the air tightness of a treatment chamber and the continuity of input and output of a conveyor belt and realize continuous film hydrophilic treatment;
(3) According to the low-temperature normal-pressure plasma surface hydrophilic modification device based on the carbon dioxide atmosphere, plasma is used for exciting carbon dioxide ionized gas ions to bombard the surface of the film to be treated, so that the surface of the film is activated. The speed of the conveyor belt is controlled, so that the film to be treated is subjected to plasma treatment in the reaction chamber for 3-5min and then is operated in the post-reaction chamber for 1min, and the sufficient bonding reaction between the activated groups on the surface of the film and ionized gas ions is ensured. Based on experiments, the surface after plasma activation is deactivated after 1-2min in air.
(4) According to the low-temperature normal-pressure plasma surface hydrophilic modification device based on the carbon dioxide atmosphere, in the pp spunbonded non-woven fabric as an example, the contact angle of the surface of the film to water can be reduced from 95 o to 32 o, so that the hydrophilic modification of the film is successfully realized. The infrared spectrometer is used for analyzing the functional groups on the surface of the film, and the absorption peaks of hydrophilic groups-OH and C-O appear on the surface of the modified PP spun-bonded non-woven fabric.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (4)
1. The low-temperature normal-pressure plasma surface hydrophilic modification device based on the carbon dioxide atmosphere is characterized by comprising a carbon dioxide gas supply unit (1), a plasma treatment chamber (2) and a conveyor belt (3);
the plasma treatment chamber (2) comprises a generation chamber (21) and a rear reaction chamber (22), wherein a positive electrode (23) and a negative electrode (24) are arranged in the generation chamber (21), the distance between the positive electrode (23) and the negative electrode (24) is 10mm-500mm, the positive electrode (23) is electrically connected with an external control power supply, the negative electrode (24) is grounded, a blower (25) is arranged at the lower left corner of the generation chamber (21) and the upper right corner of the rear reaction chamber (22), an inlet (26) is arranged at the upper left corner of the generation chamber (21), an outlet (27) is arranged at the upper right corner of the rear reaction chamber (22), the surface of a film to be treated is activated in a discharge environment when the film passes through the generation chamber, and the film after the surface treatment fully reacts with carbon dioxide gas filled in the treatment chamber in the process of passing through the rear reaction chamber to realize full reaction;
The carbon dioxide gas supply unit (1) is positioned at the top of the plasma treatment chamber (2), the bottom of the carbon dioxide gas supply unit (1) is connected with the gas pipe (11), the gas pipe (11) extends to the bottom in the generation chamber (21), a control switch (12) is arranged at the joint of the carbon dioxide gas supply unit (1) and the gas pipe (11), the control switch is electrically connected with the pressure sensor (13), and the pressure sensor (13) is positioned at the top in the generation chamber (21);
The conveyer belt (3) is U-shaped structure, and conveyer belt (3) gets into from entry (26) and takes place room (21), leaves post-reaction chamber (22) from export (27), and entry (26) and export (27) all are equipped with seal structure, and seal structure is 2 elastic silica gel piece that same direction set up, and positive electrode (23) are located the upper portion of conveyer belt (3), and negative electrode (24) are located the lower part of conveyer belt (3), and conveyer belt (3) imbeds between positive electrode (23) and negative electrode (24), and negative electrode (24) are constituteed by two at least conveying rollers, and conveying roller rotates and drives conveyer belt (3) motion, and pending film adheres to conveyer belt (3) surface.
2. The carbon dioxide atmosphere-based low-temperature atmospheric pressure plasma surface hydrophilic modification device according to claim 1, wherein the positive electrode (23) is a rod-shaped or tubular electrode, and is made of one of high-conductivity metal iron, copper and silver, the negative electrode (24) is made of stainless steel, an insulating coating is attached to the surface of the negative electrode (24), and the insulating coating is made of Al 2O3 or Ca 0.8Sr0.2TiO3.
3. A method for modifying the surface hydrophilicity of a low-temperature normal-pressure plasma based on a carbon dioxide atmosphere, which is characterized in that the device as claimed in any one of claims 1 to 2 is adopted, and the method comprises the following steps:
s1, attaching a film to be treated on a conveyor belt (3);
S2, starting a control switch, and enabling carbon dioxide in the carbon dioxide gas supply unit (1) to enter the generation chamber (21) until the pressure sensor (13) detects that the air pressure in the generation chamber (21) is equal to one atmosphere;
And S3, turning on a control power switch, discharging the positive electrode, rotating a conveying roller, driving the conveying belt (3) to move by the conveying roller, and enabling the film to be treated attached to the surface of the conveying belt (3) to sequentially pass through the generation chamber (21) and the rear reaction chamber (22).
4. The method for modifying the surface hydrophilicity of the low-temperature normal-pressure plasma based on the carbon dioxide atmosphere according to claim 3, wherein the operating power of the control power supply is 50W-50kW, the discharge frequency of the positive electrode (23) is 10kHz-100MHz, the operating time of the film to be treated in the generation chamber (21) is 3-5min, and the operating time of the post-reaction chamber (22) is 1-3min.
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