CN108311112B - Preparation method of surface sulfhydrylation carbon fiber based on low-temperature plasma technology - Google Patents
Preparation method of surface sulfhydrylation carbon fiber based on low-temperature plasma technology Download PDFInfo
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Abstract
The invention discloses a preparation method of surface sulfhydrylation carbon fiber based on a low-temperature plasma technology, and relates to the technical field of environment-friendly materials. According to the preparation method provided by the invention, carbon fibers are used as a base material, the carbon fibers are subjected to low-temperature plasma treatment under an ammonia medium to obtain the amino-enriched carbon fiber surface, and then EDC/NHS is used as a catalyst to react with sulfhydrylation reagents such as cysteine and the like in a citric acid buffer solution to obtain the surface sulfhydrylation carbon fibers with strong adsorbability, so that the technical problem of insufficient adsorbability of the carbon fibers to pollutants is solved, the technical effect of enhancing the adsorbability of the carbon fibers to the pollutants is achieved, and the preparation process of the surface sulfhydrylation modified carbon fibers is simple, low in cost and convenient for industrial production.
Description
Technical Field
The invention relates to the technical field of environment-friendly materials, in particular to a preparation method of surface sulfhydrylation carbon fiber based on a low-temperature plasma technology.
Background
The problem of environmental pollution has become a focus of attention, and heavy metal pollution in water is an extremely important environmental protection problem. Heavy metals are a class of important pollutants in the environment, and are difficult to remove from the environment once entering water and soil environments due to the characteristics of high toxicity, incapability of biodegradation, easy accumulation and the like. It can not only cause deterioration of ecological environment, but also enter food chain and cause great harm to human body. But is often discharged into rivers, lakes or oceans or enters soil after being treated to reach the standard due to certain subjective reasons or objective reasons, so that the water environment and the soil environment are polluted. The sources of heavy metal elements in water comprise wastewater generated in the mining process, wastewater generated in the dressing and smelting production process, wastewater generated in the metal processing process and wastewater generated in the electroplating process. There are many methods for removing heavy metals from water, and adsorption is one of the effective methods in common use. Therefore, in recent years, the development of novel and efficient heavy metal adsorbing materials is one of the hotspots of research in the field of environmental protection.
The carbon fiber is high-performance fiber with the carbon content of more than 90 percent, the organic fiber is carbonized at the high temperature of more than 1000 ℃, the carbon fiber material has a developed surface microporous structure and a larger specific surface area, the pore size distribution of the carbon fiber is narrow and uniform, pollutants to the aqueous solution can be removed through adsorption, the carbon fiber material has larger adsorption capacity and faster adsorption rate to organic matters, heavy metal ions and the like in the aqueous solution, and the high adsorption capacity is still maintained for low-concentration adsorbates. Therefore, the carbon fiber has wider application prospect in water treatment.
However, in the existing process of using carbon fibers to decontaminate aqueous solutions, the carbon fibers have limited adsorption capacity to organic matters, heavy metal ions and other pollutants, so the use amount of the carbon fibers is often large, and the cost for treating water pollution by using the carbon fibers is high.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of surface sulfhydrylation carbon fiber based on a low-temperature plasma technology, which is characterized in that sulfhydrylation surface modification is carried out on the carbon fiber, a sulfhydryl group is grafted to the surface of the carbon fiber, and the adsorption performance of the carbon fiber to heavy metals is improved by utilizing the coordination capacity of the sulfhydryl group.
According to an aspect of an embodiment of the present invention, there is provided a method for preparing surface-thiolated carbon fibers based on a low-temperature plasma technique, the method including:
putting the carbon fiber into a Soxhlet extractor, extracting and cleaning the carbon fiber for 24 hours at the temperature of 75 ℃ by using acetone, then cleaning the carbon fiber by using ultrapure water at the temperature of 75 ℃, and drying the carbon fiber in a drying oven at the temperature of 50 ℃;
placing the dried carbon fiber in a treatment cavity of a low-temperature plasma treatment instrument, pumping air pressure in the treatment cavity to 2-3 Pa, introducing ammonia gas for flushing, wherein the flow of the ammonia gas in the treatment cavity is 30L/min, then pumping out gas in the treatment cavity to enable the cavity of the treatment cavity to be in a vacuum state, continuously flushing the treatment cavity for 3 times by using the ammonia gas, introducing the ammonia gas into the treatment cavity again, keeping the constant pressure in the treatment cavity at 20-40 Pa, turning on a radio frequency power supply of the low-temperature plasma treatment instrument, adjusting the discharge power of the radio frequency power supply, and performing ammonia gas plasma treatment on the surface of the carbon fiber in the treatment cavity for 3-20 min, wherein the discharge power is 90-130W;
taking the carbon fiber treated by the ammonia plasma out of the treatment cavity, placing the carbon fiber in a citric acid buffer solution containing a sulfhydrylation reagent and EDC/NHS, oscillating the carbon fiber at the reaction temperature of 25-30 ℃ for 24h, filtering to obtain filter residue, washing the filter residue for 3 times by using a PBS solution, washing the filter residue by using deionized water, and placing the filter residue in a vacuum drying oven at 60 ℃ for drying to obtain the surface sulfhydrylation carbon fiber, wherein the pH of the citric acid buffer solution is adjusted to be PH =4.7 by using sodium hydroxide, the concentrations of the sulfhydrylation reagent and EDC in the citric acid buffer solution are 3-8 mg/ml, the molar ratio of EDC to NHS is 1:1, and the pH value of the PBS solution is 7.0-7.5.
In a preferred embodiment, the carbon fiber treated by the ammonia plasma is taken out of the treatment cavity and then is placed in a vacuum device for sealed storage.
In a preferred embodiment, the thiolating agent is at least one of amino acids containing a sulfhydryl group.
In a preferred embodiment, the treatment time of the ammonia plasma treatment on the surface of the carbon fiber in the treatment cavity is 15min, and the discharge power of the radio frequency power supply is 100W.
In a preferred embodiment, the concentration of the thiolating agent and EDC in the citric acid buffer solution is 5 mg/ml.
Compared with the prior art, the surface sulfhydrylation carbon fiber and the preparation method thereof provided by the invention have the following advantages:
according to the preparation method of the surface sulfhydrylation carbon fiber based on the low-temperature plasma technology, ammonia gas is selected as a reaction medium of the low-temperature plasma, so that the surface plasma etching treatment and the amination reaction process of the carbon fiber are performed simultaneously, and the modification time is saved; the carboxyl contained in the sulfhydrylation reagent such as cysteine and the like is subjected to amidation reaction with the amino on the surface of the carbon fiber, and sulfhydrylation is introduced to successfully prepare the sulfhydrylation modified carbon fiber with stronger adsorption capacity compared with the carbon fiber, so that the technical problem of insufficient adsorption capacity of the carbon fiber to pollutants is solved, the technical effect of enhancing the adsorption capacity of the carbon fiber to the pollutants is achieved, the preparation process of the surface sulfhydrylation modified carbon fiber is simple, the cost is lower, and the industrial production is facilitated.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
Fig. 1 is a flow chart illustrating a method for preparing a surface-thiolated carbon fiber based on a low-temperature plasma technique, according to an exemplary embodiment.
Detailed Description
The present invention is described in detail below with reference to specific embodiments (but not limited to) for illustration, the specific method of the embodiments is only for the purpose of illustration, the scope of the present invention is not limited by the embodiments, the present invention can be applied to various modifications and changes of various forms and structures, and these equivalents based on the present invention are also within the scope of the claims of the present invention.
Example 1
Fig. 1 illustrates a method for preparing a surface-thiolated carbon fiber based on a low-temperature plasma technique, according to an exemplary embodiment, as shown in fig. 1, the method including:
101, putting the carbon fiber into a Soxhlet extractor, extracting and cleaning the carbon fiber for 24 hours at the temperature of 75 ℃ by using acetone, cleaning the carbon fiber by using ultrapure water at the temperature of 75 ℃, and drying the carbon fiber in a drying oven at the temperature of 50 ℃.
102, placing the dried carbon fiber in a treatment cavity of a low-temperature plasma treatment instrument, pumping air pressure in the treatment cavity to 2-3 Pa, introducing ammonia gas for washing, wherein the flow rate of the ammonia gas in the treatment cavity is 30L/min, then pumping out gas in the treatment cavity, so that the cavity of the treatment cavity is in a vacuum state, continuously washing the treatment cavity for 3 times by using the ammonia gas, introducing the ammonia gas into the treatment cavity again, keeping the constant pressure in the treatment cavity at 20-40 Pa, turning on a radio frequency power supply of the low-temperature plasma treatment instrument, adjusting the discharge power of the radio frequency power supply, and performing ammonia gas plasma treatment on the surface of the carbon fiber in the treatment cavity for 3-20 min, wherein the discharge power is 90-130W.
Of these, EDC/NHS was used as a catalyst and was collectively referred to as 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride (EDC)/N-hydroxysuccinimide (NHS).
In the low-temperature gas discharge plasma, also called plasma-enhanced chemical vapor deposition, chemical bonds of volatile gaseous monomers are broken in a high-energy state of current discharge, and the volatile gaseous monomers are covalently bonded and recombined on the surface of a material, so that active functional layers with different structures and chemical compositions are formed on the surface.
The invention adopts ammonia gas as the reaction medium of low-temperature plasma, so that the action depth of the preparation process on the carbon fiber is only hundreds of angstroms, the basic property of the carbon fiber material is not influenced, and the preparation process has stronger sterilization effect while modifying the surface of the carbon fiber.
In a preferred embodiment, the carbon fiber treated by the ammonia plasma is taken out of the treatment cavity and then is placed in a vacuum device for sealed storage.
The sealing is performed to prevent the surface of the carbon fiber from being contaminated and corroded by other gases in the air.
In a preferred embodiment, the thiolating agent is at least one of amino acids containing a sulfhydryl group.
For example, the thiolating agent is cysteine.
In a preferred embodiment, the treatment time of the ammonia plasma treatment on the surface of the carbon fiber in the treatment cavity is 15min, and the discharge power of the radio frequency power supply is 100W.
In a preferred embodiment, the concentration of the thiolating agent and EDC in the citric acid buffer solution is 5 mg/ml.
According to the preparation method of the surface sulfhydrylation carbon fiber based on the low-temperature plasma technology, ammonia gas is selected as a reaction medium of the low-temperature plasma, so that the surface plasma etching treatment and the amination reaction process of the carbon fiber are performed simultaneously, and the modification time is saved; the carboxyl contained in the sulfhydrylation reagent such as cysteine and the like is subjected to amidation reaction with the amino on the surface of the carbon fiber, and sulfhydrylation is introduced to successfully prepare the sulfhydrylation modified carbon fiber with stronger adsorption capacity compared with the carbon fiber, so that the technical problem of insufficient adsorption capacity of the carbon fiber to pollutants is solved, the technical effect of enhancing the adsorption capacity of the carbon fiber to the pollutants is achieved, the preparation process of the surface sulfhydrylation modified carbon fiber is simple, the cost is lower, and the industrial production is facilitated.
Example 2
(1) Putting the carbon fiber into a Soxhlet extractor, extracting and cleaning the carbon fiber for 24 hours by acetone at the temperature of 75 ℃, then cleaning the carbon fiber by ultrapure water at the temperature of 75 ℃, and drying the carbon fiber in a drying oven at the temperature of 50 ℃.
(2) Placing the dried carbon fibers in a treatment cavity of a low-temperature plasma treatment instrument, pumping air pressure in the treatment cavity to 2Pa, introducing ammonia gas for flushing, wherein the flow of the ammonia gas in the treatment cavity is 30L/min, then pumping out gas in the treatment cavity, so that the cavity of the treatment cavity is in a vacuum state, continuously flushing the treatment cavity with the ammonia gas for 3 times, introducing the ammonia gas into the treatment cavity again, keeping the constant pressure in the treatment cavity at 20Pa, turning on a radio-frequency power supply of the low-temperature plasma treatment instrument, adjusting the discharge power of the radio-frequency power supply, and performing ammonia plasma treatment on the surfaces of the carbon fibers in the treatment cavity for 15min with the discharge power of 120W.
(3) Taking the carbon fiber treated by the ammonia plasma out of the treatment cavity, placing the carbon fiber in a citric acid buffer solution containing cysteine and EDC/NHS, shaking the carbon fiber at the reaction temperature of 25 ℃ for 24 hours, filtering the carbon fiber to obtain filter residue, washing the filter residue for 3 times by using PBS (phosphate buffer solution), washing the filter residue by using deionized water, placing the filter residue in a vacuum drying oven at the temperature of 60 ℃ for drying to prepare the surface-thiolated carbon fiber, adjusting the pH of the citric acid buffer solution to be =4.7 by using sodium hydroxide, wherein the concentrations of the cysteine and the EDC in the citric acid buffer solution are 3mg/ml, the molar ratio of the EDC to the NHS is 1:1, and the pH value of the PBS is 7.0.
Example 3
(1) Putting the carbon fiber into a Soxhlet extractor, extracting and cleaning the carbon fiber for 24 hours by acetone at the temperature of 75 ℃, then cleaning the carbon fiber by ultrapure water at the temperature of 75 ℃, and drying the carbon fiber in a drying oven at the temperature of 50 ℃.
(2) Placing the dried carbon fibers in a treatment cavity of a low-temperature plasma treatment instrument, pumping air pressure in the treatment cavity to 3Pa, introducing ammonia gas for flushing, wherein the flow of the ammonia gas in the treatment cavity is 30L/min, then pumping out gas in the treatment cavity, so that the cavity of the treatment cavity is in a vacuum state, continuously flushing the treatment cavity for 3 times by using the ammonia gas, introducing the ammonia gas into the treatment cavity again, keeping the constant pressure in the treatment cavity at 30Pa, turning on a radio-frequency power supply of the low-temperature plasma treatment instrument, adjusting the discharge power of the radio-frequency power supply, and performing ammonia plasma treatment on the surfaces of the carbon fibers in the treatment cavity for 15min with the discharge power of 100W.
(3) Taking the carbon fiber treated by the ammonia plasma out of the treatment cavity, placing the carbon fiber in a citric acid buffer solution containing cysteine and EDC/NHS, shaking the carbon fiber at the reaction temperature of 28 ℃ for 24 hours, filtering the carbon fiber to obtain filter residue, washing the filter residue for 3 times by using PBS (phosphate buffer solution), washing the filter residue by using deionized water, placing the filter residue in a vacuum drying oven at the temperature of 60 ℃ for drying to prepare the surface-thiolated carbon fiber, adjusting the pH of the citric acid buffer solution to be =4.7 by using sodium hydroxide, wherein the concentrations of the cysteine and the EDC in the citric acid buffer solution are 5mg/ml, the molar ratio of the EDC to the NHS is 1:1, and the pH value of the PBS is 7.3.
Example 4
(1) Putting the carbon fiber into a Soxhlet extractor, extracting and cleaning the carbon fiber for 24 hours by acetone at the temperature of 75 ℃, then cleaning the carbon fiber by ultrapure water at the temperature of 75 ℃, and drying the carbon fiber in a drying oven at the temperature of 50 ℃.
(2) Placing the dried carbon fiber in a treatment cavity of a low-temperature plasma treatment instrument, pumping air pressure in the treatment cavity to 3Pa, introducing ammonia gas for flushing, wherein the flow of the ammonia gas in the treatment cavity is 30L/min, then pumping out gas in the treatment cavity, so that the cavity of the treatment cavity is in a vacuum state, continuously flushing the treatment cavity for 3 times by using the ammonia gas, introducing the ammonia gas into the treatment cavity again, keeping the constant pressure in the treatment cavity at 40Pa, turning on a radio frequency power supply of the low-temperature plasma treatment instrument, adjusting the discharge power of the radio frequency power supply, and performing ammonia plasma treatment on the surface of the carbon fiber in the treatment cavity, wherein the treatment time is 20min, and the discharge power is 130W.
(3) Taking the carbon fiber treated by the ammonia plasma out of the treatment cavity, placing the carbon fiber in a citric acid buffer solution containing cysteine and EDC/NHS, shaking the carbon fiber at the reaction temperature of 30 ℃ for 24 hours, filtering the carbon fiber to obtain filter residue, washing the filter residue for 3 times by using PBS (phosphate buffer solution), washing the filter residue by using deionized water, placing the filter residue in a vacuum drying oven at the temperature of 60 ℃ for drying to prepare the surface-thiolated carbon fiber, adjusting the pH of the citric acid buffer solution to be =4.7 by using sodium hydroxide, wherein the concentrations of the cysteine and the EDC in the citric acid buffer solution are 8mg/ml, the molar ratio of the EDC to the NHS is 1:1, and the pH value of the PBS is 7.5.
Effect testing
1. Test standard
1) The performance tests of the above examples 2 to 4 were performed, and the test items were the adsorption effects of heavy metal ions such as Pb, Cd, Cr, and Cu, and the specific test methods were as follows:
the surface thiolated carbon fiber prepared in each example and the existing carbon fiber are respectively placed in the same water body environment for 12 hours and then taken out, and the adsorption effect of each example on heavy metal ions such as Pb, Cd, Cr and Cu is tested and calculated.
Analysis of test results
Table 1 shows the results of testing the adsorption effect of the surface-thiolated carbon fibers prepared in examples 2 to 4 and comparative examples on heavy metal ions of Pb, Cd, Cr and Cu.
TABLE 1 Performance test results for surface-thiolated carbon fibers
As can be seen from Table 1, the adsorption effect of the surface-thiolated carbon fibers prepared in examples 2 to 4 on heavy metal ions such as Pb, Cd, Cr and Cu is better than that of the comparative examples, wherein the adsorption effect of the surface-thiolated carbon fibers prepared in example 2 on heavy metal ions such as Pb, Cd, Cr and Cu is better than that of the other examples. According to experimental results, the preparation method of the surface sulfhydrylation carbon fiber based on the low-temperature plasma technology provided by the embodiment of the invention can greatly improve the adsorption performance of the carbon fiber to heavy metals by performing sulfhydrylation surface modification on the carbon fiber, grafting a sulfhydryl group to the surface of the carbon fiber and utilizing the matching capacity of the sulfhydryl group.
The invention provides a preparation method of surface sulfhydrylation carbon fiber based on low-temperature plasma technology, which comprises the steps of firstly carrying out amination modification on the surface of the carbon fiber by adopting the plasma technology, then further reacting the product with a sulfhydrylation reagent to obtain the surface sulfhydrylation carbon fiber, and preparing the surface sulfhydrylation carbon fiber with strong adsorption capacity by the two steps, wherein the preparation process is simple and the production cost is low.
While the invention has been described in detail in the foregoing by way of general description, and specific embodiments and experiments, it will be apparent to those skilled in the art that modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This invention is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It will be understood that the invention is not limited to the precise arrangements described above and shown in the drawings and that various modifications and changes may be made without departing from the scope thereof.
Claims (5)
1. A method for preparing surface sulfhydrylation carbon fiber based on low-temperature plasma technology is characterized by comprising the following steps:
putting the carbon fiber into a Soxhlet extractor, extracting and cleaning the carbon fiber for 24 hours at the temperature of 75 ℃ by using acetone, then cleaning the carbon fiber by using ultrapure water at the temperature of 75 ℃, and drying the carbon fiber in a drying oven at the temperature of 50 ℃;
placing the dried carbon fiber in a treatment cavity of a low-temperature plasma treatment instrument, pumping air pressure in the treatment cavity to 2-3 Pa, introducing ammonia gas for flushing, wherein the flow of the ammonia gas in the treatment cavity is 30L/min, then pumping out gas in the treatment cavity to enable the cavity of the treatment cavity to be in a vacuum state, continuously flushing the treatment cavity for 3 times by using the ammonia gas, introducing the ammonia gas into the treatment cavity again, keeping the constant pressure in the treatment cavity at 20-40 Pa, turning on a radio frequency power supply of the low-temperature plasma treatment instrument, adjusting the discharge power of the radio frequency power supply, and performing ammonia gas plasma treatment on the surface of the carbon fiber in the treatment cavity for 3-20 min, wherein the discharge power is 90-130W;
taking the carbon fiber treated by the ammonia plasma out of the treatment cavity, placing the carbon fiber in a citric acid buffer solution containing a sulfhydrylation reagent and EDC/NHS, oscillating the carbon fiber at the reaction temperature of 25-30 ℃ for 24h, filtering to obtain filter residue, washing the filter residue for 3 times by using a PBS solution, washing the filter residue by using deionized water, placing the filter residue in a vacuum drying oven at 60 ℃ for drying to prepare the surface sulfhydrylation carbon fiber, adjusting the pH of the citric acid buffer solution to be =4.7 by using sodium hydroxide, wherein the concentrations of the sulfhydrylation reagent and EDC in the citric acid buffer solution are 3-8 mg/mL, the molar ratio of EDC to NHS is 1:1, and the pH value of the PBS solution is 7.0-7.5.
2. The method according to claim 1, wherein the carbon fiber treated by the ammonia plasma is taken out of the treatment chamber and then is hermetically stored in a vacuum device.
3. The method of claim 1, wherein the thiolating agent is at least one of amino acids containing a sulfhydryl group.
4. The method according to claim 1, wherein the treatment time of ammonia plasma treatment on the surface of the carbon fiber in the treatment cavity is 15min, and the discharge power of the radio frequency power supply is 100W.
5. The method of claim 1, wherein the concentration of thiolating agent and EDC in the citric acid buffer solution is 5 mg/mL.
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