CN107325303B - Degumming-free silk fiber solution, preparation method and application thereof - Google Patents

Degumming-free silk fiber solution, preparation method and application thereof Download PDF

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CN107325303B
CN107325303B CN201710641443.2A CN201710641443A CN107325303B CN 107325303 B CN107325303 B CN 107325303B CN 201710641443 A CN201710641443 A CN 201710641443A CN 107325303 B CN107325303 B CN 107325303B
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degumming
silk
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free silk
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CN107325303A (en
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刘志
徐珍珍
赵江惠
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Anhui Polytechnic University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
    • C08J3/11—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids from solid polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/74—Natural macromolecular material or derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4266—Natural fibres not provided for in group D04H1/425
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2389/00—Characterised by the use of proteins; Derivatives thereof

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Organic Chemistry (AREA)
  • Hydrology & Water Resources (AREA)
  • Water Supply & Treatment (AREA)
  • Environmental & Geological Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Artificial Filaments (AREA)
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Abstract

The invention discloses a degumming-free silk fiber solution, a preparation method and application thereof, wherein the preparation method comprises the following steps: dissolving inorganic salt in organic acid to prepare a mixed solvent A, wherein the mass ratio of the inorganic salt to the organic acid is 0.5-10: 100; and step two, placing the degumming-free silk in the mixed solvent A, and stirring the degumming-free silk at normal temperature to obtain a transparent solution. The invention can directly dissolve the degumming-free silk fiber, does not need to consume a large amount of water and various chemical medicines in the degumming process, and the degumming wastewater causes adverse effects on the environment.

Description

Degumming-free silk fiber solution, preparation method and application thereof
Technical Field
The invention belongs to the technical field of natural organic polymers, and particularly relates to a degumming-free silk solution, a preparation method and application thereof.
Background
The silk fiber is composed of two main components of sericin and silk fibroin. As a natural organic polymer material, the material has the advantages of excellent rebound resilience, moisture absorption and the like and is widely used in the field of clothing. In recent years, regenerated silk materials have been used in the biomedical field and the like due to good biocompatibility and excellent mechanical properties of silk fibers. In the application of the biological medicine field, sericin has adverse inflammatory reaction to human body. Therefore, in the biomedical field, it is more common to use the regenerated silk fibroin solution after degumming. Therefore, the dissolution method of degummed silk fibroin is generally reported in the literature and patents at present.
However, the mechanical properties of the regenerated silk material are reduced after degumming. The reason for this is that, first: the natural silk is composed of sericin and silk fibroin, one sericin is wrapped outside the two silk fibroin, the unique bonding structure of the two silk fibroin is the main reason of the excellent mechanical property of the natural silk, and only silk fibroin is left after degumming, so that the mechanical property of the regenerated material is inevitably affected; secondly, the method comprises the following steps: it is known from literature that The stronger The degree of degumming, The poorer The mechanical properties of recycled materials (Dou H, Zuo B. The Journal of The Textile Institute,2015,106(3): 311-. Therefore, it is expected that the mechanical properties of the non-degummed regenerated silk fiber material will be improved to a large extent.
The traditional dissolving method is to carry out degumming process. The degumming process needs a large amount of water and Na2CO3And the like. The sericin/chemical agent aqueous solution after being removed is directly discharged, which causes adverse effect on the environment. The silk fibroin after degumming is dissolved in high concentration inorganic salt water solution system, such as LiBr water solution (Lock, R L. process for making silk fibroin fibers [ P ]].US Patent:5252285,1993-10-20.)、 CaCl2Ethanol/water ternary solvents (Li M Z, Zhang C S, Lu S Z, et al. polymers for Advanced Technologies,2002,13(8):605-10), and the like. After degumming, a dialysis process is required, which also requires a large amount of water and expensive dialysis bags, and a dialysis process of more than three days is required. Finally, the regenerated fibroin solution is obtained. Therefore, the traditional method for dissolving the degummed silk fibroin has complex process, time consumption and high cost. Furthermore, these dissolution methods have not been investigated for direct dissolution of degumless silk fibres.
A dissolving system newly developed in recent years mainly comprises N-methyl-N-morpholine oxide (NMMO) (Shangying, Shaohuili, Chaochen super, Henan university institute of university (Nature edition), 2004,32(1):45-51.) and ionic liquid (Shao Zheng, Wang celery, Yangyu, fibroin ionic liquid solution preparation method: CN, CN102153766A [ P ]. 2011.). The NMMO system has limited dissolving capacity to silk fibroin, and the dissolving temperature is as high as more than 90 ℃. The silk fibroin can be dissolved by the ionic liquid generally by heating, and the requirements on the dissolving conditions are strict, such as avoiding moisture, needing nitrogen protection and the like. Likewise, these dissolution methods have not been investigated for direct dissolution of degumless silk fibres.
CN 106589091 a discloses a "dissolving method of natural silk fiber", which is to dissolve degummed silk fibroin by using acid and inorganic salt to obtain a silk fibroin regeneration solution. However, silk fibers contain small amounts of oils, waxes, pectins, etc. in addition to silk fibroin and sericin. The acid and inorganic salt system cannot know whether the degumming-free silk fiber can be directly dissolved. Therefore, the present invention has not been discussed yet for the direct dissolution of degumless silk fibres.
Therefore, the direct dissolution of the degumming-free silk fiber is the first and key problem for expanding the application of the regenerated silk protein material to wider high and new technical fields. However, no method for directly dissolving silk fibers has been reported so far.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a degumming-free silk solution, a preparation method and application thereof, aiming at directly dissolving degumming-free silk fiber and greatly improving the mechanical property of a regenerated silk fiber material obtained by subsequent application.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a degumming-free silk fiber solution comprises the following steps:
dissolving inorganic salt in organic acid to prepare a mixed solvent A, wherein the mass ratio of the inorganic salt to the organic acid is 0.5-10: 100;
and step two, placing the degumming-free silk in the mixed solvent A, and stirring the degumming-free silk at normal temperature to obtain a transparent solution.
The inorganic salt is halogen inorganic salt, and the organic acid is formic acid or trifluoroacetic acid. The mixed solvent composed of the inorganic salt and the organic acid is reasonably selected, so that the degumming-free silk has a better dissolving effect.
The halogen inorganic salt is one or more of calcium chloride, magnesium chloride or lithium bromide.
The halogen inorganic salt is calcium chloride, and the organic acid is formic acid. The inorganic salt in the mixed solvent is calcium chloride, and the organic acid is formic acid, so that the dissolving efficiency is high, and the cost is low.
The degumming-free silk is one or more of mulberry silk, tussah silk and castor-oil plant silk.
The mass percentage of the silk fiber in the total solution is 0.1-15%. The silk fibre dissolving process of this content is easy to carry out, and the silk fibre of higher content will make the dissolving process very difficult.
A degumming-free silk fiber solution is prepared by the above method.
The invention also provides an application of the degumming-free silk fiber solution, which is used for preparing the degumming-free silk nanofiber membrane through an electrostatic spinning process.
The invention also provides the application of the degumming-free silk nanofiber membrane, which is used for the pretreatment of wastewater filtration and food concentration. The regenerated fibroin filtering membrane has better mechanical property. In addition, the silk protein has good biocompatibility and natural hydrophilic property, so that the regenerated degumming-free silk protein filter membrane has wide application prospect in the field of filtration, separation and concentration.
The invention has the beneficial effects that:
1. the invention can directly dissolve the degumming-free silk fiber, does not need to consume a large amount of water and various chemical medicines in the degumming process, and the degumming wastewater causes adverse effects on the environment.
2. The mechanical property of the regenerated silk fiber material prepared by the invention is greatly improved, and the application of the regenerated silk protein material is facilitated, particularly the pretreatment of the waste water filtration field and the food concentration.
3. The process for dissolving the degumming-free silk fiber is simple, and the regenerated silk protein solution can be obtained at normal temperature. High dissolving efficiency, low cost and practical application value.
Drawings
The description includes the following figures, the contents shown are respectively:
FIG. 1 is an optical picture of a degumming-free silk fiber solution according to the present invention;
FIG. 2 is an SEM image of a degumming-free silk nanofiber microfilm according to the present invention.
Detailed Description
The following detailed description of the embodiments of the present invention will be given with reference to the accompanying drawings for a purpose of helping those skilled in the art to more fully, accurately and deeply understand the concept and technical solution of the present invention and to facilitate its implementation.
A preparation method of a degumming-free silk fiber solution comprises the following steps:
dissolving inorganic salt in organic acid to prepare a mixed solvent A, wherein the mass ratio of the inorganic salt to the organic acid is 0.5-10: 100; the inorganic salt can be one or more of calcium chloride, magnesium chloride or lithium bromide; the organic acid is formic acid or trifluoroacetic acid;
and step two, placing the degumming-free silk in the mixed solvent A, and stirring the degumming-free silk at normal temperature to obtain a transparent solution.
Wherein, the inorganic salt and the organic acid can be matched at will to prepare a mixed solvent. The inorganic salt is preferably CaCl in consideration of dissolution efficiency and cost2The organic acid is preferably formic acid.
The degumming-free silk fiber solution obtained by the preparation method can be used for obtaining regenerated silk nanofiber membranes, regenerated silk filaments, regenerated silk films and the like through different processing technologies.
In the process of preparing the regenerated silk nanofiber membrane and the like, the mass percentage of the silk fibers in the total solution is preferably 0.1-15%.
The following is illustrated in detail by specific examples:
example 1
A preparation method of a degumming-free silk fiber solution comprises the following steps:
step one, weighing 0.05 g of degumming-free silk, washing with deionized water and drying for later use.
Weighing 0.2 g of anhydrous CaCl2The resulting mixture was dissolved in 20 g of anhydrous formic acid to prepare a mixed solvent. Stirring at normal temperature to obtain a transparent solution.
And step three, placing the dried degumming-free silk in a prepared mixed solvent. Stirring at normal temperature to obtain transparent solution (figure 1), which is regenerated degumming-free fibroin solution.
Through the electrostatic spinning process, the regenerated degumming-free silk solution is poured into an injector, and the regenerated silk nanofiber membrane (shown in figure 2) is obtained under the conditions that the applied voltage is 25kV and the receiving distance is 20 cm.
Example 2
A preparation method of a degumming-free silk fiber solution comprises the following steps:
step one, weighing 0.1 g of degumming-free silk, washing with deionized water and drying for later use.
Weighing 0.2 g of anhydrous CaCl2Dissolving in 20 g of anhydrous formic acid to prepare a mixed solvent, and stirring at normal temperature to obtain a transparent solution.
And step three, placing the dried degumming-free silk into a prepared mixed solvent, and stirring the mixture at normal temperature to obtain a transparent solution, namely the regenerated degumming-free silk protein solution.
Pouring the regenerated degumming-free silk solution into an injector through an electrostatic spinning process, and obtaining the regenerated silk nanofiber membrane under the conditions of applying voltage of 20kV and receiving distance of 15 cm.
Example 3
A preparation method of a degumming-free silk fiber solution comprises the following steps:
step one, weighing 0.2 g of degumming-free silk, washing with deionized water and drying for later use.
Weighing 0.2 g of anhydrous CaCl2Dissolving in 20 g of anhydrous formic acid to prepare a mixed solvent, and stirring at normal temperature to obtain a transparent solution.
And step three, placing the dried degumming-free silk into a prepared mixed solvent, and stirring the mixture at normal temperature to obtain a transparent solution, namely the regenerated degumming-free silk protein solution.
Pouring the regenerated degumming-free silk solution into an injector through an electrostatic spinning process, and obtaining the regenerated silk nanofiber membrane under the conditions of applying voltage of 25kV and receiving distance of 30 cm.
Example 4
A preparation method of a degumming-free silk fiber solution comprises the following steps:
step one, weighing 0.2 g of degumming-free silk, washing with deionized water and drying for later use.
And step two, weighing 0.2 g of anhydrous LiBr, dissolving in 20 g of anhydrous formic acid, preparing a mixed solvent, and stirring at normal temperature to obtain a transparent solution.
And step three, placing the dried degumming-free silk into a prepared mixed solvent, and stirring the mixture at normal temperature to obtain a transparent solution, namely the regenerated degumming-free silk protein solution.
Pouring the regenerated degumming-free silk solution into an injector through an electrostatic spinning process, and obtaining the regenerated silk nanofiber membrane under the conditions of applying voltage of 25kV and receiving distance of 30 cm.
Example 5
A preparation method of a degumming-free silk fiber solution comprises the following steps:
step one, weighing 0.2 g of degumming-free silk, washing with deionized water and drying for later use.
Weighing 0.2 g of anhydrous CaCl2Dissolving in 20 g of trifluoroacetic acid to prepare a mixed solvent, and stirring at normal temperature to obtain a transparent solution.
And step three, placing the dried degumming-free silk into a prepared mixed solvent, and stirring the mixture at normal temperature to obtain a transparent solution, namely the regenerated degumming-free silk protein solution.
Pouring the regenerated degumming-free silk solution into an injector through an electrostatic spinning process, and obtaining the regenerated silk nanofiber membrane under the conditions of applying voltage of 25kV and receiving distance of 30 cm.
Example 6
A preparation method of a degumming-free silk fiber solution comprises the following steps:
step one, weighing 0.4 g of degumming-free silk, washing with deionized water and drying for later use.
Weighing 0.2 g of anhydrous CaCl2Dissolving in 20 g of trifluoroacetic acid to prepare a mixed solvent, and stirring at normal temperature to obtain a transparent solution.
And step three, placing the dried degumming-free silk into a prepared mixed solvent, and stirring the mixture at normal temperature to obtain a transparent solution, namely the regenerated degumming-free silk protein solution.
And pouring the regenerated degumming-free silk limiting solution into a glass vessel or a plastic vessel, and drying at normal temperature in a ventilated kitchen until formic acid is completely volatilized to obtain the regenerated silk film.
Example 7
The difference between this example and example 6 is that 0.2 g of degumming-free silk was weighed in step one.
Example 8
This example is different from example 1 in that 0.1 g of anhydrous CaCl was weighed in the second step2。
Example 9
The difference between this example and example 1 is that in step one, 1g of degumming-free silk was weighed, and in step two, 0.07 g of anhydrous CaCl was weighed2In 7g of anhydrous formic acid.
Example 10
This example is different from example 9 in that in the second step, 0.07 g MgCl was weighed2In 7g of anhydrous formic acid.
Example 11
The difference between this example and example 1 is that in step one, 1g of degumming-free silk was weighed, and in step two, 30g of anhydrous formic acid was weighed.
Through the experimental process of the above examples, it was found that the same amount of CaCl was weighed2And formic acid is used as a mixed solvent to dissolve the degumming-free silk, and the dissolving efficiency of the mixed solvent prepared by other inorganic salts and organic acid is relatively higher. The dissolution efficiency of example 11 was not as good as that of example 1. In addition, CaCl2And formic acid is used as a mixed solvent, the material cost is relatively low, and the regenerated silk nanofiber membrane and the regenerated silk film prepared from the regenerated degumming-free silk fiber solution obtained by dissolving have better mechanical properties.
The invention is described above with reference to the accompanying drawings. It is to be understood that the specific implementations of the invention are not limited in this respect. Various insubstantial improvements are made by adopting the method conception and the technical scheme of the invention; the present invention is not limited to the above embodiments, and can be modified in various ways.

Claims (1)

1. A preparation method of a degumming-free silk fiber solution is characterized by comprising the following steps:
dissolving inorganic salt in organic acid to prepare a mixed solvent A, wherein the mass ratio of the inorganic salt to the organic acid is 0.5-1: 100;
step two, placing the non-degummed silk in the mixed solvent A, and stirring the mixture at normal temperature to obtain a transparent solution;
the inorganic salt is anhydrous calcium chloride, and the organic acid is anhydrous formic acid; the mass percentage of the non-degummed silk fiber in the total solution is 0.1-15%;
the degumming-free silk is one or more of mulberry silk, tussah silk and castor-oil plant silk.
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CN109161975B (en) * 2018-09-18 2021-02-02 南京林业大学 PH-sensitive fibroin nanofiber, and dispersion liquid, preparation method and application thereof
CN111333458A (en) * 2020-05-07 2020-06-26 安徽肥地肥业有限责任公司 Method for preparing organic fertilizer containing nicotine
CN113249876A (en) * 2021-06-10 2021-08-13 上海科技大学 Ion conductor material and preparation method and application thereof
CN113279282A (en) * 2021-06-25 2021-08-20 陕西科技大学 Silk-reinforced aramid nanofiber film and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN106367816A (en) * 2016-11-18 2017-02-01 辽东学院 Method for high-temperature and high-pressure acid degumming of tussah silk
CN106436304A (en) * 2016-11-18 2017-02-22 辽东学院 Silk-gum and organic-acid finishing liquid and method thereof for skin-close finishing on cotton fabric
CN106589091A (en) * 2016-12-09 2017-04-26 宁波芸生纺织品科技有限公司 Method for dissolving fiber of natural silk

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106367816A (en) * 2016-11-18 2017-02-01 辽东学院 Method for high-temperature and high-pressure acid degumming of tussah silk
CN106436304A (en) * 2016-11-18 2017-02-22 辽东学院 Silk-gum and organic-acid finishing liquid and method thereof for skin-close finishing on cotton fabric
CN106589091A (en) * 2016-12-09 2017-04-26 宁波芸生纺织品科技有限公司 Method for dissolving fiber of natural silk

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