CN108277635B - Preparation method of surface sulfhydrylation silk fiber based on low-temperature plasma technology - Google Patents
Preparation method of surface sulfhydrylation silk fiber based on low-temperature plasma technology Download PDFInfo
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- CN108277635B CN108277635B CN201810217651.4A CN201810217651A CN108277635B CN 108277635 B CN108277635 B CN 108277635B CN 201810217651 A CN201810217651 A CN 201810217651A CN 108277635 B CN108277635 B CN 108277635B
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- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
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- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/08—Organic compounds
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
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Abstract
The invention discloses a preparation method of surface sulfhydrylation silk fibers 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, ammonia gas is selected as a reaction medium of low-temperature plasma, so that the surface plasma etching treatment and the amination reaction process of the silk fiber are simultaneously carried out, the modification time is saved, and the amidation reaction is carried out between carboxyl contained in sulfhydrylation reagents such as cysteine and the amino on the surface of the silk fiber, so that the modification effect of the silk fiber is stable, the adsorption effect of the prepared surface sulfhydrylation silk fiber is stronger and stable, the technical problem that the adsorption effect is unstable when the heavy metal adsorption material is prepared from the silk fiber is solved, the technical effect of using the silk fiber to produce the adsorption material with strong and stable heavy metal adsorption capacity is achieved, the application range of the silk fiber is widened, the preparation process of the surface sulfhydrylation modification silk fiber is simple, and the cost is lower.
Description
Technical Field
The invention relates to the technical field of environment-friendly materials, in particular to a preparation method of surface sulfhydrylation silk fibers 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, wastewater generated in the electroplating process and the like. 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 silk fiber is a natural fiber widely used in China, has a typical natural protein structure and is composed of at least 18 amino acids. The silk fiber is environment-friendly, has the characteristics of large surface area, easiness in physical and chemical modification and the like, and is an ideal carrier, however, a certain amount of amino acid is distributed on the surface of unmodified silk, but the total content of free amino and carboxyl is not large, so that the adsorption capacity of the silk fiber on heavy metal ions is not high, and the silk fiber cannot be directly used for adsorbing heavy metals.
The existing method for preparing the heavy metal adsorbing material by modifying silk comprises the following steps: (1) pretreatment: putting the raw silk of the current year silkworm into a weak alkaline solution, adding lipase, alkaline protease and surfactant, treating with ultrasonic waves, soaking, boiling, and washing with water; (2) constant weight: putting the cleaned silk into a freeze drying box for drying, then weighing the dried silk, and then carrying out freeze drying and weighing; (3) and (3) detection: sampling silk with constant weight, and detecting the silk by using a picric acid carmine reagent; (4) modification: and (3) directly soaking the fibroin into a neutral protease solution, treating with ultrasonic waves, and freeze-drying to constant weight to obtain the required adsorbing material.
The inventor finds that the method for preparing the heavy metal adsorption material from the silk needs to adopt multiple enzymes for treatment, the silk fiber is modified by the neutral protease solution, the activity of the enzymes has instability and is easily influenced by external environmental factors such as temperature and air, and the activity of the enzymes is easily influenced after multiple soaking, so that the modification effect of the silk fiber is greatly influenced in the actual operation process, and the prepared adsorption material has poor actual adsorption effect on the heavy metals.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of surface sulfhydrylation silk fiber based on low-temperature plasma technology, which is characterized in that sulfhydrylation surface modification is carried out on the silk fiber, a sulfhydryl group is grafted to the surface of the silk fiber, and the adsorption performance of the silk fiber to heavy metals is improved by utilizing the matching capability of the sulfhydryl group.
According to an aspect of the embodiments of the present invention, there is provided a method for preparing surface thiolated silk fibers based on a low-temperature plasma technology, the method including:
placing silk fibers in an anhydrous sodium carbonate solution at the temperature of 97-98 ℃ for degumming treatment for 1h, then sending the degummed silk fibers into warm water for cleaning, dewatering and drying, wherein the bath ratio of the silk fibers to the anhydrous sodium carbonate solution is 1: 100, and the mass concentration of anhydrous sodium carbonate in the anhydrous sodium carbonate solution is 5 g/L;
placing the dehydrated and dried silk fibers in a treatment cavity of a low-temperature plasma treatment instrument, pumping system air pressure in the treatment cavity to 2-3 Pa, introducing ammonia gas for washing, 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 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 surfaces of the silk fibers in the treatment cavity for 3-20 min, wherein the discharge power is 90-130W;
the silk fiber after being treated by ammonia plasma is taken out of the treatment cavity, placed in a citric acid buffer solution containing a sulfhydrylation reagent and EDC/NHS, shaken at the reaction temperature of 25-30 ℃ for 24h and then filtered to obtain filter residue, the filter residue is washed for 3 times by a PBS solution, and then washed by deionized water, the filter residue is placed in a vacuum drying oven at 60 ℃ to be dried to prepare the surface sulfhydrylation silk fiber, the pH of the citric acid buffer solution is adjusted to be PH =4.7 by 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 silk fiber after being treated by the ammonia plasma is taken out of the treatment cavity and is placed in a vacuum device for sealed preservation.
In a preferred embodiment, the silk fiber is at least one of mulberry silk or tussah silk.
In a preferred embodiment, the thiolating agent is at least one of amino acids having a sulfhydryl group.
In a preferred embodiment, the treatment time of the ammonia plasma treatment on the silk fiber surface in the treatment cavity is 10min, 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 6 mg/ml.
Compared with the prior art, the surface sulfhydrylation silk fiber and the preparation method thereof provided by the invention have the following advantages:
the method for preparing the surface thiolated silk fiber based on the low-temperature plasma technology has the advantages that ammonia gas is selected as a reaction medium of the low-temperature plasma, so that the etching treatment and the amination reaction processes of the surface plasma of the silk fiber are simultaneously performed, the modification time is saved, the amidation reaction is performed between carboxyl contained in a thiolated reagent such as cysteine and the like and amino on the surface of the silk fiber, so that the modification effect of the silk fiber is stable, the adsorption effect of the prepared surface thiolated silk fiber is strong and stable, the technical problem that the adsorption effect is unstable when the silk fiber is used for preparing a heavy metal adsorption material is solved, the technical effect of using the silk fiber to produce the adsorption material with strong and stable heavy metal adsorption capacity is achieved, the application range of the silk fiber is widened, and the preparation process of the surface thiolated modified silk fiber is simple, the cost is low, and the industrial production is convenient.
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 shows a method for preparing surface-thiolated silk fibers 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 shows a method for preparing surface-thiolated silk fibers based on a low-temperature plasma technique, according to an exemplary embodiment, as shown in fig. 1, the method including:
101, placing silk fibers in an anhydrous sodium carbonate solution at the temperature of 97-98 ℃ for degumming treatment for 1h, then sending the silk fibers subjected to degumming treatment into warm water for cleaning, dewatering and drying, wherein the bath ratio of the silk fibers to the anhydrous sodium carbonate solution is 1: 100, and the mass concentration of anhydrous sodium carbonate in the anhydrous sodium carbonate solution is 5 g/L.
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).
The invention adopts ammonia gas as a medium of the low-temperature plasma, can stably and efficiently modify silk fibers, and can quickly realize the conversion from the silk fibers to heavy metal adsorption materials.
In a preferred embodiment, the silk fiber after being treated by the ammonia plasma is taken out of the treatment cavity and is placed in a vacuum device for sealed preservation.
The sealing preservation is to prevent the surface of the silk fiber after treatment from being polluted and corroded by other gases in the air.
The silk fiber includes at least one of mulberry silk and tussah silk.
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 silk fiber surface in the treatment cavity is 10min, 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 6 mg/ml.
The method for preparing the surface thiolated silk fiber based on the low-temperature plasma technology has the advantages that ammonia gas is selected as a reaction medium of the low-temperature plasma, so that the etching treatment and the amination reaction processes of the surface plasma of the silk fiber are simultaneously performed, the modification time is saved, the amidation reaction is performed between carboxyl contained in a thiolated reagent such as cysteine and the like and amino on the surface of the silk fiber, so that the modification effect of the silk fiber is stable, the adsorption effect of the prepared surface thiolated silk fiber is strong and stable, the technical problem that the adsorption effect is unstable when the silk fiber is used for preparing a heavy metal adsorption material is solved, the technical effect of using the silk fiber to produce the adsorption material with strong and stable heavy metal adsorption capacity is achieved, the application range of the silk fiber is widened, and the preparation process of the surface thiolated modified silk fiber is simple, the cost is low, and the industrial production is convenient.
Example 2
(1) Placing silk fibers in an anhydrous sodium carbonate solution at the temperature of 97 ℃ for degumming treatment for 1h, then sending the silk fibers into warm water for cleaning, dewatering and drying after degumming treatment, wherein the bath ratio of the silk fibers to the anhydrous sodium carbonate solution is 1: 100, and the mass concentration of anhydrous sodium carbonate in the anhydrous sodium carbonate solution is 5 g/L.
(2) After will dewatering and drying silk fibre is arranged in the process chamber of low temperature plasma processing appearance, will system atmospheric pressure in the process chamber is taken out and is let in the ammonia and wash after 2Pa, the ammonia is in the flow of process chamber is 30L/min, then will the gas in the process chamber is taken out, makes in the vacuum state in the process chamber, it is right to use the ammonia in succession the process chamber washes 3 backs, once more to the process chamber lets in the ammonia, and keeps the constant 20Pa of pressure in the process chamber, opens the radio frequency power supply of low temperature plasma processing appearance, and adjusts radio frequency power supply's discharge power, right in the process chamber silk fibre surface carries out ammonia plasma and handles, and processing time is 10min, and discharge power is 100W.
(3) The silk fiber after ammonia plasma treatment is taken out of the treatment cavity, placed in a vacuum device for sealed preservation, then placed in a citric acid buffer solution containing cysteine and EDC/NHS, shaken for 24h at the reaction temperature of 25 ℃ and filtered to obtain filter residue, the filter residue is washed for 3 times by PBS solution, and then is washed by deionized water, and the filter residue is dried by placing the filter residue in a vacuum drying box at 60 ℃ to prepare the surface thiolated silk fiber, wherein the citric acid buffer solution is adjusted to PH =4.7 by sodium hydroxide, the concentrations of the cysteine and the EDC in the citric acid buffer solution are 6mg/ml, the molar ratio of the EDC to the NHS is 1:1, and the PH value of the PBS solution is 7.0.
Example 3
(1) Placing silk fibers in an anhydrous sodium carbonate solution at the temperature of 97 ℃ for degumming treatment for 1h, then sending the silk fibers into warm water for cleaning, dewatering and drying after degumming treatment, wherein the bath ratio of the silk fibers to the anhydrous sodium carbonate solution is 1: 100, and the mass concentration of anhydrous sodium carbonate in the anhydrous sodium carbonate solution is 5 g/L.
(2) After will dewatering and drying silk fibre is arranged in the process chamber of low temperature plasma processing appearance, will the system atmospheric pressure of process chamber is taken out and is let in the ammonia and wash after 3Pa, the ammonia is in the flow of process chamber is 30L/min, then will the gas of process chamber is taken out, makes in the vacuum state in the process chamber cavity, it is right to use the ammonia in succession the process chamber washes 3 backs, once more to the process chamber lets in the ammonia, and keeps the constant 30Pa of pressure in the process chamber cavity, opens the radio frequency power supply of low temperature plasma processing appearance, and adjusts radio frequency power supply's discharge power, right in the process chamber silk fibre surface carries out ammonia plasma and handles, and processing time is 3min, and discharge power is 90W.
(3) The silk fiber after ammonia plasma treatment is taken out of the treatment cavity, placed in a vacuum device for sealed preservation, then placed in a citric acid buffer solution containing cysteine and EDC/NHS, shaken for 24h at the reaction temperature of 28 ℃ and filtered to obtain filter residue, the filter residue is washed for 3 times by PBS solution, and then is washed by deionized water, the filter residue is dried by placing in a vacuum drying box at 60 ℃ after being washed, the surface thiolated silk fiber is prepared, the citric acid buffer solution is adjusted to PH =4.7 by sodium hydroxide, the concentrations of the cysteine and the EDC in the citric acid buffer solution are 6mg/ml, the molar ratio of the EDC to the NHS is 1:1, and the PH value of the PBS solution is 7.3.
Example 4
(1) Placing silk fibers in an anhydrous sodium carbonate solution at the temperature of 98 ℃ for degumming for 1h, then sending the silk fibers subjected to degumming into warm water for cleaning, dewatering and drying, wherein the bath ratio of the silk fibers to the anhydrous sodium carbonate solution is 1: 100, and the mass concentration of anhydrous sodium carbonate in the anhydrous sodium carbonate solution is 5 g/L.
(2) After will dewatering and drying silk fibre is arranged in the process chamber of low temperature plasma processing appearance, will system atmospheric pressure in the process chamber is taken out and is let in the ammonia and wash after 3Pa, the ammonia is in the flow of process chamber is 30L/min, then will the gas in the process chamber is taken out, makes in the vacuum state in the process chamber, it is right to use the ammonia in succession the process chamber washes 3 backs, once more to the process chamber lets in the ammonia, and keeps the constant 40Pa of pressure in the process chamber, opens the radio frequency power supply of low temperature plasma processing appearance, and adjusts radio frequency power supply's discharge power, right in the process chamber silk fibre surface carries out ammonia plasma and handles, and processing time is 20min, and discharge power is 130W.
(3) The silk fiber after ammonia plasma treatment is taken out of the treatment cavity, placed in a vacuum device for sealed preservation, then placed in a citric acid buffer solution containing cysteine and EDC/NHS, shaken at the reaction temperature of 30 ℃ for 24h and then filtered to obtain filter residue, washed for 3 times by PBS solution, and then washed by deionized water, and then dried by placing the filter residue in a vacuum drying box at 60 ℃ to prepare the surface thiolated silk fiber, wherein the citric acid buffer solution is adjusted to PH =4.7 by sodium hydroxide, 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 solution 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:
and (3) respectively placing the surface thiolated silk fiber prepared in each embodiment and the existing carbon fiber in the same water body environment for 12 hours, then taking out, and testing and calculating the adsorption effect of each embodiment on heavy metal ions such as Pb, Cd, Cr and Cu.
Analysis of test results
Table 1 shows the results of testing the adsorption effect of the surface-thiolated silk 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 Silk fibers
As can be seen from table 1, the adsorption effect of the surface-thiolated silk 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, and the adsorption effect of the surface-thiolated silk 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 the preparation method of the surface sulfhydrylation silk fiber, provided by the embodiment of the invention, the sulfhydrylation surface modification is carried out on the silk fiber, so that a sulfhydryl group is grafted to the surface of the silk fiber, the adsorption performance of the sulfhydrylation silk fiber on heavy metals can be improved by utilizing the matching capacity of the sulfhydryl group, and the application field range of the silk fiber is widened.
The preparation method of the surface sulfhydrylation silk fiber based on the low-temperature plasma technology can restore the pollution of heavy metals to the environment, and meets the requirements of environmental protection, energy conservation and resource conservation.
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 preparation method of surface thiolated silk fibers based on a low-temperature plasma technology is characterized by comprising the following steps:
placing silk fibers in an anhydrous sodium carbonate solution at the temperature of 97-98 ℃ for degumming treatment for 1h, then sending the degummed silk fibers into warm water for cleaning, dewatering and drying, wherein the bath ratio of the silk fibers to the anhydrous sodium carbonate solution is 1: 100, and the mass concentration of anhydrous sodium carbonate in the anhydrous sodium carbonate solution is 5 g/L;
placing the dehydrated and dried silk fibers in a treatment cavity of a low-temperature plasma treatment instrument, pumping system air pressure in the treatment cavity to 2-3 Pa, introducing ammonia gas for washing, 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 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 surfaces of the silk fibers in the treatment cavity for 3-20 min, wherein the discharge power is 90-130W;
the silk fiber treated by ammonia plasma is taken out of the treatment cavity, placed in a citric acid buffer solution containing a sulfhydrylation reagent and EDC/NHS, shaken at the reaction temperature of 25-30 ℃ for 24h and then filtered to obtain filter residue, the filter residue is washed for 3 times by PBS solution, then washed by deionized water, and then dried in a vacuum drying oven at 60 ℃ to prepare the surface sulfhydrylation silk fiber, the pH of the citric acid buffer solution is adjusted to be pH =4.7 by 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, the pH value of the PBS solution is 7.0-7.5, and the sulfhydrylation reagent is at least one of amino acids containing sulfhydryl groups.
2. The method according to claim 1, wherein the silk 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 according to claim 1, wherein the silk fibers are at least one of mulberry silk or tussah silk.
4. The method according to claim 1, wherein the ammonia plasma treatment is performed on the silk fiber surface in the treatment cavity for 10min, and the discharge power of the radio frequency power supply is 100W.
5. The method of claim 1, wherein the concentration of the thiolating agent and EDC in the citric acid buffer solution is 6 mg/ml.
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