CN115073795A - Hydrophobic polymer material surface hydrophilic modification method based on carbon dioxide plasma - Google Patents
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Abstract
本发明公开了一种基于二氧化碳等离子体的疏水性聚合物材料表面亲水改性方法，该方法包括：步骤一：采用高压空气等离子体喷枪将等离子体射流喷射于疏水性聚合物材料表面，得到清洗后的疏水性聚合物材料；步骤二：将清洗后的疏水性聚合物材料置于等离子体处理装置中，将等离子体处理装置抽真空，然后通入第一混合气体，控制气体流量，调节等离子体处理装置内的气压，当等离子体处理装置内的气压稳定后，启动电源，对聚合物材料表面进行等离子体改性处理，得到预改性材料；步骤三：关闭等离子体处理装置的电源，将预改性材料在等离子体处理装置中静置，即得。该发明的方法处理后的聚合物材料表面具有良好的亲水性，还能实现二氧化碳的活化再利用。
The invention discloses a method for hydrophilic modification of the surface of a hydrophobic polymer material based on carbon dioxide plasma. The method comprises: step 1: using a high-pressure air plasma spray gun to spray a plasma jet on the surface of the hydrophobic polymer material to obtain The cleaned hydrophobic polymer material; step 2: placing the cleaned hydrophobic polymer material in a plasma processing device, evacuating the plasma processing device, and then introducing the first mixed gas, controlling the gas flow, adjusting the The air pressure in the plasma treatment device, when the air pressure in the plasma treatment device is stable, start the power supply, and perform plasma modification treatment on the surface of the polymer material to obtain a pre-modified material; Step 3: Turn off the power supply of the plasma treatment device , and the pre-modified material is allowed to stand in the plasma treatment device, that is, it is obtained. The surface of the polymer material treated by the method of the invention has good hydrophilicity, and can also realize the activation and reuse of carbon dioxide.
Description
Technical Field
The invention relates to the technical field of material modification, in particular to a carbon dioxide plasma-based hydrophilic modification method for the surface of a hydrophobic polymer material.
Background
The plasma surface treatment technology is to excite gas molecules by certain energy, so that the gas is dissociated into excited states such as electrons, ions, free radicals and other metastable states, and the excited states collide with the surface of a material to destroy covalent bonds, generate free radicals and activate the surface of the material. And the activated material surface can be combined with an excited gas to generate chemical active groups on the surface. The plasma surface treatment technology is widely applied to the industries of electroplating, coating and printing ink at present, and the binding force between the plasma surface treatment technology and a base material is increased. Some researchers have performed plasma modification on the bamboo surface by using plasma, and found that the contact angle of the bamboo surface to water can be effectively reduced by plasma treatment, but the contact angle surface can be slowly recovered with the time. Applicants have also studied plasma technology encapsulation and have found that plasma can activate the surface of any substance, but the activated groups annihilate over time. Therefore, in order to obtain a material surface with good hydrophilicity, some researchers use a plasma grafting technology to graft-polymerize a hydrophilic monomer or polymer on a hydrophobic surface activated by plasma, and the obtained material surface has a low contact angle. Han et al treated the feldspar ceramic with the vapor generated after atmospheric pressure helium plasma ionized triethylene glycol dimethacrylate, and the results show that the ceramic surface after plasma jet treatment contains hydroxyl radicals and the hydrophilicity is improved.
Carbon dioxide is a very stable molecule and is relatively difficult to excite and then react. Global warming caused by the emission of greenhouse gases mainly containing carbon dioxide is seriously threatening the survival and sustainable development of human beings, and is one of the major global challenges facing human beings at present. Meanwhile, the task of improving the environmental quality at the present stage in China is still serious, and in recent years, a lot of research is focused on the adsorption and energy regeneration of carbon dioxide. Among them, the research of catalytically decomposing carbon dioxide by plasma technology has become one of the hot spots of research of energy regeneration of carbon dioxide, but the conversion rate of carbon monoxide or methane obtained at present is not ideal, and the utilization rate of carbon dioxide is not high. It has been found that carbon dioxide is activated as an electron acceptor, and the decomposition efficiency of carbon dioxide can be improved to some extent by blending carbon dioxide with a rare gas such as oxygen or argon. The polymer material loses electrons after being bombarded by ions, generates a plurality of activated groups, and is favorable for the activated carbon dioxide to be covalently bonded with the surface of the material while accelerating the decomposition of the carbon dioxide, so that permanent hydrophilic groups are formed on the surface of the material. The method aims to activate and reuse the carbon dioxide, generate more hydrophilic groups on the surface of the material, and reduce the emission of the carbon dioxide in the environment.
Disclosure of Invention
The invention aims to provide a vacuum plasma surface hydrophilic modification technology in a carbon dioxide atmosphere, which ionizes carbon dioxide by using high-frequency electricity, can realize hydrophilic modification of the surface of a hydrophobic polymer film, realizes reutilization of carbon dioxide, and reduces emission of carbon dioxide.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a carbon dioxide plasma-based hydrophilic modification method for the surface of a hydrophobic polymer material, which comprises the following steps:
the method comprises the following steps: spraying plasma jet on the surface of the hydrophobic polymer material by using a high-pressure air plasma spray gun to obtain the cleaned hydrophobic polymer material;
step two: placing the cleaned hydrophobic polymer material in a plasma processing device, vacuumizing the plasma processing device, introducing a first mixed gas, controlling the gas flow, adjusting the gas pressure in the plasma processing device, starting a power supply after the gas pressure in the plasma processing device is stable, and performing plasma modification treatment on the surface of the polymer material to obtain a pre-modified material;
step three: and (3) closing the power supply of the plasma processing device, and standing the pre-modified material in the plasma processing device to obtain the modified material.
Further, in the second step, the first mixed gas comprises carbon dioxide and a second mixed gas, and the volume ratio of the second mixed gas to the carbon dioxide is (0-5): (95-100).
Further, the second mixed gas is oxygen or a rare gas.
Further, in the second step, the vacuum degree is pumped to 5-10Pa, the time of modification treatment is 3-10min, the pressure of modification treatment is 20-80Pa, and the power supply power of the plasma treatment device is 50-300W.
Further, in the third step, the standing time of the pre-modified material in the plasma processing device is 30s-3 min.
Further, the hydrophobic polymer material includes polyethylene, polypropylene, polyesters, silicone.
Compared with the prior art, the invention has the beneficial effects that:
the surface of the polymer material treated by the plasma has good hydrophilicity, and the method is used in the fields of super absorbent materials, biomedical materials, oil-water separation and the like. And the surface of the modified polymer material has good hydrophilic stability, and the contact angle does not change obviously along with the time. Compared with the existing plasma surface modification technology, the method does not need a polymer monomer, is not easy to generate pollution, and can realize the activation and reutilization of carbon dioxide, thereby reducing the storage of the carbon dioxide in the environment. The method has short reaction time and good modification effect in the modification process.
Drawings
FIG. 1 is a schematic diagram showing the modified effect of example 1;
FIG. 2 is a schematic diagram showing the modified effect of example 3;
FIG. 3 is a schematic diagram showing the modified effect of example 4.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a carbon dioxide plasma-based hydrophilic modification method for the surface of a hydrophobic polymer material, which comprises the following steps:
the method comprises the following steps: spraying plasma jet on the surface of the hydrophobic polymer material by using a high-pressure air plasma spray gun to obtain the cleaned hydrophobic polymer material;
step two: placing the cleaned hydrophobic polymer material in a plasma processing device, vacuumizing the plasma processing device, introducing a first mixed gas, controlling the gas flow, adjusting the gas pressure in the plasma processing device, starting a high-frequency power supply after the gas pressure in the plasma processing device is stable, and performing plasma modification treatment on the surface of the polymer material to obtain a pre-modified material;
step three: and (3) closing a high-frequency power supply of the plasma processing device, and standing the pre-modified material in the plasma processing device to obtain the modified material.
Specifically, in the second step, the first mixed gas includes carbon dioxide and a second mixed gas, and the volume ratio of the second mixed gas to the carbon dioxide is (0-5): (95-100).
Specifically, the second mixed gas is oxygen or a rare gas.
Specifically, in the second step, the vacuum degree is pumped to 5-10Pa, the time of modification treatment is 3-10min, the pressure of modification treatment is 20-80Pa, and the power supply power of the plasma treatment device is 50-300W.
Specifically, in the third step, the pre-modified material is kept still in the plasma processing device for 30s-3 min.
Specifically, the hydrophobic polymer material includes a film, a rod-like or three-dimensional material, such as polyethylene, polypropylene, polyesters, silica gel, and rubber.
Example 1
The embodiment discloses a carbon dioxide plasma-based hydrophobic polymer material surface hydrophilic modification method, which comprises the following steps:
s1: the polypropylene spunbonded non-woven fabric is placed on an operation table, a high-pressure atmospheric plasma spray gun capable of moving in two dimensions at the speed of 5m/min is adopted, plasma jet flow is sprayed on the surface of the polypropylene spunbonded non-woven fabric, and the polypropylene spunbonded non-woven fabric is cleaned under the conditions that the voltage is 200V and the discharge frequency is 15 kHz.
S2: the cleaned polypropylene spun-bonded nonwoven is arranged in a plasma processing device, the plasma processing device is pumped to the vacuum degree of 5Pa, and CO is introduced 2 The gas pressure in the plasma processing apparatus was adjusted to 40 Pa. And starting the high-frequency power supply after the stabilization, wherein the processing power is 300W, and the processing time is 5 min.
S3: the high-frequency power supply is turned off, the polypropylene spun-bonded non-woven fabric is taken out after 1min to obtain modified polypropylene, and the contact angle of the modified polypropylene is measured to be reduced from 97.5 degrees before treatment to 48.5 degrees. After one month, the contact angle was measured to be 49.9 ° as shown in fig. 1.
Example 2
The embodiment discloses a carbon dioxide plasma-based hydrophobic polymer material surface hydrophilic modification method, which comprises the following steps:
placing the ultra-high molecular weight polyethylene rod-shaped material on an operation table, and moving up and down at a speed of 10m/min，15 o The high-pressure atmospheric plasma spray gun rotating at/min sprays plasma jet on the surface of the ultra-high molecular weight polyethylene rod-shaped material, and the ultra-high molecular weight polyethylene rod is cleaned under the conditions that the voltage is 200V and the discharge frequency is 15 kHz.
Placing the cleaned ultra-high molecular weight polyethylene rod in a plasma processing device, pumping the plasma processing device to the vacuum degree of 5Pa, and introducing CO 2 And O 2 Mixed gas of (2), wherein O 2 The volume ratio of the water-soluble organic silicon compound is 5 percent. The pressure in the plasma processing apparatus was adjusted to 80 Pa. And starting the high-frequency power supply after the stabilization, wherein the processing power is 250W, and the processing time is 10 min.
And (3) turning off the high-frequency power supply, taking out the ultra-high molecular weight polyethylene rod after 3min to obtain a modified ultra-high molecular weight polyethylene rod, immersing the modified ultra-high molecular weight polyethylene rod in water, and taking out the modified ultra-high molecular weight polyethylene rod to obtain a relatively uniform water film, wherein liquid drops cannot flow down in strands.
Example 3
The embodiment discloses a hydrophobic polymer material surface hydrophilic modification method based on carbon dioxide plasma, which comprises the following steps:
s1: the polyester foam is placed on an operation table, a high-pressure atmospheric plasma spray gun capable of moving in two dimensions at the speed of 5m/min is adopted, plasma jet is sprayed on the surface of the polyester foam, and the polyester foam is cleaned under the conditions that the voltage is 200V and the discharge frequency is 15 kHz.
S2: placing the cleaned polyester foam in a plasma processing device, pumping the plasma processing device to the vacuum degree of 7Pa, and introducing CO 2 And O 2 Mixed gas of (2), wherein O 2 The occupied volume ratio is 2 percent. The pressure in the plasma processing apparatus was adjusted to 20 Pa. And starting the high-frequency power supply after the stabilization, wherein the processing power is 50W, and the processing time is 10 min.
S3: the high-frequency power supply is turned off, the polyester foam is taken out after 3min, and the contact angle of the polyester foam is measured to be reduced from 90 degrees to 38.4 degrees. After one month, the contact angle was measured to be 37 ° as shown in fig. 2.
Example 4
The embodiment discloses a carbon dioxide plasma-based hydrophobic polymer material surface hydrophilic modification method, which comprises the following steps:
s1: the polytetrafluoroethylene plate is placed on an operation table, a normal-pressure atmospheric plasma spray gun capable of moving in two dimensions at the speed of 1m/min is adopted, plasma jet flow is sprayed on the surface of the polytetrafluoroethylene plate, and polyester foam is cleaned under the conditions that the voltage is 200V and the discharge frequency is 15 kHz.
S2: placing the cleaned polyester foam in a plasma processing device, pumping the plasma processing device to the vacuum degree of 5Pa, and introducing CO 2 And O 2 Mixed gas of (2), wherein O 2 The occupied volume ratio is 1 percent. The pressure in the plasma processing apparatus was adjusted to 60 Pa. And starting a high-frequency power supply after the stabilization, wherein the processing power is 300W, and the processing time is 8 min.
S3: the high-frequency power supply is turned off, the polyester foam is taken out after 3min, and the contact angle of the polyester foam is measured to be reduced from 103 degrees to 64 degrees. After one month, the contact angle was measured to be 68 ° as shown in fig. 3.
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 attributes 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 description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (6)
1. A method for hydrophilic modification of the surface of a hydrophobic polymer material based on carbon dioxide plasma is characterized by comprising the following steps:
the method comprises the following steps: spraying plasma jet on the surface of the hydrophobic polymer material by using a high-pressure air plasma spray gun to obtain the cleaned hydrophobic polymer material;
step two: placing the cleaned hydrophobic polymer material in a plasma processing device, vacuumizing the plasma processing device, introducing a first mixed gas, controlling the gas flow, adjusting the gas pressure in the plasma processing device, starting a power supply after the gas pressure in the plasma processing device is stable, and performing plasma modification treatment on the surface of the polymer material to obtain a pre-modified material;
step three: and (3) closing the power supply of the plasma treatment device, and standing the pre-modified material in the plasma treatment device to obtain the modified material.
2. The method for hydrophilic modification of the surface of hydrophobic polymer material based on carbon dioxide plasma according to claim 1, wherein in the second step, the first mixed gas comprises carbon dioxide and a second mixed gas, and the volume ratio of the second mixed gas to the carbon dioxide is (0-5): (95-100).
3. The method for hydrophilic modification of the surface of hydrophobic polymer material based on carbon dioxide plasma as claimed in claim 2, wherein the second mixed gas is oxygen or rare gas.
4. The method for hydrophilic modification of the surface of hydrophobic polymer material based on carbon dioxide plasma according to claim 1, wherein in the second step, vacuum is applied until the vacuum degree is 5-10Pa, the time of the modification treatment is 3-10min, the pressure of the modification treatment is 20-80Pa, and the power supply of the plasma treatment device is 50-300W.
5. The method for hydrophilic modification of the surface of hydrophobic polymer material based on carbon dioxide plasma according to claim 1, wherein in the third step, the pre-modified material is left in the plasma treatment device for 30s-3 min.
6. The method for hydrophilic modification of the surface of a hydrophobic polymer material based on carbon dioxide plasma as claimed in claim 1, wherein the hydrophobic polymer material comprises polyethylene, polypropylene, polyester, silica gel, and rubber, and the form of the hydrophobic polymer material is thin film, rod or three-dimensional structure.
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Cited By (2)
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| CN119932914A (en) * | 2024-12-16 | 2025-05-06 | 中国石油化工股份有限公司 | Oil-water separation material and preparation method thereof |
| CN121397847A (en) * | 2025-10-30 | 2026-01-23 | 上海玄电新材料有限公司 | Plasma-assisted surface activation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN119932914A (en) * | 2024-12-16 | 2025-05-06 | 中国石油化工股份有限公司 | Oil-water separation material and preparation method thereof |
| CN121397847A (en) * | 2025-10-30 | 2026-01-23 | 上海玄电新材料有限公司 | Plasma-assisted surface activation method |
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