CN113913956A - Micro-fluidic spinning construction method for high-strength spiral fibers - Google Patents
Micro-fluidic spinning construction method for high-strength spiral fibers Download PDFInfo
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- CN113913956A CN113913956A CN202111134964.1A CN202111134964A CN113913956A CN 113913956 A CN113913956 A CN 113913956A CN 202111134964 A CN202111134964 A CN 202111134964A CN 113913956 A CN113913956 A CN 113913956A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/22—Formation of filaments, threads, or the like with a crimped or curled structure; with a special structure to simulate wool
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/14—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated alcohols, e.g. polyvinyl alcohol, or of their acetals or ketals
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
- D01F6/625—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters derived from hydroxy-carboxylic acids, e.g. lactones
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/70—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyurethanes
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/76—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from other polycondensation products
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Abstract
The invention relates to a micro-fluidic spinning construction method of high-strength spiral fibers. The method comprises the following specific steps: dissolving a polymer in a solvent to prepare a uniform solution to obtain a spinning solution; then, adopting a coaxial capillary microfluidic chip, taking the spinning solution obtained in the step A as an inner phase, taking a coagulant as an outer phase, and controlling the flow velocity of the inner phase and the flow velocity of the outer phase through a microfluidic pump to carry out microfluidic spinning; and finally, collecting the spiral fiber obtained in the step B through a winding device. The method is based on the difference of Hansen solubility parameters of polymers in different solvents, and the polymer solution and the coagulating bath are subjected to solvent exchange, so that the viscosity of the polymer solution is increased, phase separation is carried out, and finally fibers are spiralized. The invention breaks through the limitation of raw materials for constructing the spiral fiber by the traditional method, adopts various polymers to construct the high-strength spiral fiber, such as polycaprolactone, polyvinyl alcohol, polyvinyl butyral, polysulfone, polyether sulfone and the like, improves the strength of the spiral fiber material, and has universality.
Description
Technical Field
The invention relates to a micro-fluidic spinning construction method of high-strength spiral fibers.
Background
Helical structures are widely found in nature, such as DNA double helix structures, plant vines, and the like. Compared with the traditional rigid material, the spiral structure fiber has higher deformation capability, thereby showing the characteristics of high elasticity, high flexibility and the like, and having huge application potential in the fields of tissue engineering, artificial skin, biomedicine and the like. The micro-fluidic spinning technology has the characteristics of high specific surface area, high heat and mass transfer efficiency, accurate and controllable fiber structure, continuity and the like, and is widely applied to the macro preparation of functional anisotropic micro-nano fibers, particularly spiral fibers. By coupling PEGDA with a sodium alginate-calcium chloride system, professor Zhaojinjin of southeast university couples the PEGDA with the sodium alginate-calcium chloride system, prepares calcium alginate spiral fiber through the ionic crosslinking between calcium ions and carboxylate radicals, and then initiates the PEGDA in the fiber to generate chemical crosslinking through ultraviolet light, a spiral micro-motor can be constructed (Angewandte chemical-International Edition 2017,56, 12127-. Professor li bin, university of suzhou, constructed hollow helical fibers for artificial blood vessels using a sodium alginate-calcium chloride system (adv. healthcare mater.2019,8,1900435).
Although the research on the construction of spiral fibers by the micro-fluidic spinning technology is greatly advanced at home and abroad, the strength of the fibers is still low, and the reason for the low strength is limited by the preparation principle and raw materials of the spiral fibers. The raw materials for constructing the spiral fiber by traditional microfluidic spinning are usually limited to sodium alginate, polyethylene glycol diacrylate, chitosan or glucan and the like, and the fiber is formed based on the principle of ionic crosslinking or chemical crosslinking. The inherent nature of the raw material results in a product with low strength of the spiral fiber, limiting its development and application.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a microfluidic spinning construction method of high-strength spiral fibers, and the technical problem to be solved is the limitation of the traditional microfluidic spinning construction of spiral fiber raw materials, mainly limited to sodium alginate, polyethylene glycol diacrylate, chitosan or glucan and the like. Due to the limitation of the inherent properties of the material, the strength of the spiral fiber product is low, and the application requirements of multiple fields are difficult to meet. The method is based on the difference of Hansen solubility parameters of polymers in different solvents, and the polymer solution and the coagulating bath are subjected to solvent exchange, so that the viscosity of the polymer solution is increased, phase separation is carried out, and finally fibers are spiralized. The invention breaks through the limitation of raw materials for constructing the spiral fiber by the traditional method, adopts various polymers to construct the high-strength spiral fiber, improves the strength of the spiral fiber material and has universality.
The technical scheme of the invention is as follows: a micro-fluidic spinning construction method of high-strength spiral fibers comprises the following specific steps:
A. dissolving a polymer in a solvent to prepare a uniform solution to obtain a spinning solution;
B. adopting a coaxial capillary microfluidic chip, taking the spinning solution obtained in the step A as an inner phase, taking a coagulant as an outer phase, and controlling the flow velocity of the inner phase and the flow velocity of the outer phase through a digital microfluidic pump to carry out microfluidic spinning;
C. and C, adjusting an included angle between the microfluidic chip and the horizontal plane, and collecting the spiral fiber obtained in the step B through a winding device.
Preferably, the polymer material in step a is polycaprolactone, polyurethane, polyvinyl butyral, polysulfone, polyethersulfone or polyvinyl alcohol.
Preferably, the solvent in step A is at least one of formic acid, dichloromethane, N-dimethylformamide, dimethyl sulfoxide or ethanol.
Preferably, the mass concentration of the spinning solution in the step A is 10-25%.
Preferably, the diameter of the phase outlet in the coaxial capillary microfluidic chip in the step B is 100-200 μm.
Preferably, the coagulant in step B is at least one of water, methanol, ethanol, dimethyl sulfoxide and N, N-dimethylformamide.
Preferably, the flow rate of the inner phase in the step B is 1-5 mL/h, and the flow rate of the outer phase is 10-50 mL/h.
Preferably, the included angle between the microfluidic chip in the step C and the horizontal plane is 0-90 degrees.
In order to achieve the purpose, the invention designs a universal micro-fluidic spinning construction method of the high-strength spiral fiber, and the high-strength spiral fiber with a controllable structure is obtained by continuously debugging process parameters.
Has the advantages that:
(1) the invention can be widely applied to various polymers, such as polycaprolactone, polyurethane, polyvinyl butyral, polysulfone, polyethersulfone, polyvinyl alcohol and the like, and breaks through the limitation of raw materials in the traditional method.
(2) The invention solves the problems of low strength and the like of the spiral fiber prepared by the traditional method, and provides a feasible method for preparing the high-strength spiral fiber.
(3) The invention provides a basis for the macro production of the functional high-strength spiral fiber.
Drawings
FIG. 1 is an optical micrograph of a spiral fiber obtained in example 1;
FIG. 2 is an optical micrograph of a spiral fiber obtained in example 2;
FIG. 3 is an optical micrograph of a spiral fiber obtained in example 3;
FIG. 4 is an optical micrograph of a spiral fiber obtained in example 4;
FIG. 5 is an optical micrograph of a spiral fiber obtained in example 5;
FIG. 6 is an optical micrograph of a spiral fiber obtained in example 6;
FIG. 7 is an optical micrograph of a spiral fiber obtained in example 7.
Detailed Description
The present invention will be described below with reference to specific examples, but the present invention is not limited to the following examples.
Example 1
Dissolving polycaprolactone in formic acid to prepare spinning solution with the mass fraction of 10%. A coaxial capillary micro-fluidic chip with an inner phase outlet inner diameter of 100 mu m and an outer phase inner diameter of 1mm is adopted, spinning liquid is used as an inner phase, water is used as an outer phase, and the inner phase flow rate is controlled to be 1mL/h and the outer phase flow rate is controlled to be 10mL/h through a digital micro-fluidic pump. And adjusting the included angle between the microfluidic chip and the horizontal plane to be 0 degree, collecting the obtained spiral fiber through a winding device, and carrying out appearance and performance tests. The optical micrograph of the obtained spiral fiber is shown in FIG. 1, and it can be seen that the diameter of the spiral fiber is 68 μm, the pitch is 474 μm, and the amplitude is 243 μm. Tensile strength results are shown in Table 1 below, from which it can be seen that the resulting helical fiber has a tensile strength of 25.1 MPa.
Example 2
Dissolving polycaprolactone in dichloromethane to prepare spinning solution with the mass fraction of 10%. A coaxial capillary micro-fluidic chip with an inner phase outlet inner diameter of 150 mu m and an outer phase inner diameter of 1mm is adopted, spinning solution is used as an inner phase, methanol is used as an outer phase, and the inner phase flow rate is controlled to be 2.5mL/h and the outer phase flow rate is controlled to be 25mL/h through a digital micro-fluidic pump. And adjusting the included angle of the microfluidic chip and the horizontal plane to be 30 degrees, collecting the obtained spiral fiber through a winding device, and carrying out appearance and performance tests. The optical micrograph of the obtained spiral fiber is shown in FIG. 2, and it can be seen that the spiral fiber had a diameter of 80 μm, a pitch of 578 μm, and an amplitude of 291 μm. Tensile strength results are shown in Table 1 below, from which it can be seen that the resulting helical fiber has a tensile strength of 23 MPa.
Example 3
And (3) dissolving polyurethane in N, N-dimethylformamide to prepare a spinning solution with the mass fraction of 15%. A coaxial capillary micro-fluidic chip with an inner phase outlet inner diameter of 180 mu m and an outer phase inner diameter of 1mm is adopted, spinning solution is used as an inner phase, a mixed solution (mass ratio is 1:1) of N, N-dimethylformamide and water is used as an outer phase, the inner phase flow rate is controlled to be 3mL/h through a digital micro-fluidic pump, and the outer phase flow rate is controlled to be 30 mL/h. And adjusting the included angle between the microfluidic chip and the horizontal plane to be 60 degrees, collecting the obtained spiral fiber through a winding device, and carrying out appearance and performance tests. The optical micrograph of the obtained spiral fiber is shown in FIG. 3, and it can be seen that the spiral fiber had a diameter of 112 μm, a pitch of 826 μm and an amplitude of 419. mu.m. Tensile strength results are shown in Table 1 below, from which it can be seen that the resulting helical fiber has a tensile strength of 27.5 MPa.
Example 4
And dissolving the polyvinyl butyral in dimethyl sulfoxide to prepare a spinning solution with the mass fraction of 15%. A coaxial capillary microfluidic chip with the inner phase outlet diameter of 140 mu m and the outer phase inner diameter of 1mm is adopted, spinning solution is used as the inner phase, a mixed solution of dimethyl sulfoxide and water (the mass ratio is 3:1) is used as the outer phase, the inner phase flow rate is controlled to be 3mL/h through a digital microfluidic control, and the outer phase flow rate is controlled to be 30 mL/h. And adjusting the included angle between the microfluidic chip and the horizontal plane to be 0 degree, collecting the obtained spiral fiber through a winding device, and carrying out appearance and performance tests. The optical micrograph of the obtained spiral fiber is shown in FIG. 4, and it can be seen that the diameter of the spiral fiber was 100. mu.m, the pitch was 689 μm, and the amplitude was 423 μm. Tensile strength results are shown in Table 1 below, from which it can be seen that the resulting helical fiber has a tensile strength of 20 MPa.
Example 5
Dissolving polysulfone in dimethyl sulfoxide to prepare spinning solution with the mass fraction of 20%. A coaxial capillary microfluidic chip with the inner phase outlet diameter of 140 mu m and the outer phase inner diameter of 1mm is adopted, spinning solution is used as the inner phase, a mixed solution of dimethyl sulfoxide and water (the mass ratio is 3:1) is used as the outer phase, the inner phase flow rate is controlled to be 3mL/h through a digital microfluidic control, and the outer phase flow rate is controlled to be 30 mL/h. And adjusting the included angle between the microfluidic chip and the horizontal plane to be 0 degree, collecting the obtained spiral fiber through a winding device, and carrying out appearance and performance tests. The optical micrograph of the obtained spiral fiber is shown in FIG. 5, and it can be seen that the diameter of the spiral fiber was 106 μm, the pitch was 506 μm, and the amplitude was 401 μm. Tensile strength results are shown in Table 1 below, from which it can be seen that the resulting helical fiber tensile strength is 13.7 MPa.
Example 6
Dissolving polyether sulfone in dimethyl sulfoxide to prepare spinning solution with the mass fraction of 25%. A coaxial capillary microfluidic chip with the inner phase outlet diameter of 140 mu m and the outer phase inner diameter of 1mm is adopted, spinning solution is used as the inner phase, a mixed solution of dimethyl sulfoxide and water (the mass ratio is 3:1) is used as the outer phase, the inner phase flow rate is controlled to be 3mL/h through a digital microfluidic control, and the outer phase flow rate is controlled to be 30 mL/h. And adjusting the included angle between the microfluidic chip and the horizontal plane to be 0 degree, collecting the obtained spiral fiber through a winding device, and carrying out appearance and performance tests. The optical micrograph of the obtained spiral fiber is shown in FIG. 6, and it can be seen that the spiral fiber had a diameter of 104 μm, a pitch of 795 μm, and an amplitude of 419. mu.m. Tensile strength results are shown in Table 1 below, from which it can be seen that the resulting helical fiber has a tensile strength of 23.5 MPa.
Example 7
And (3) dissolving polyvinyl alcohol in dimethyl sulfoxide to prepare spinning solution with the mass fraction of 10%. A coaxial capillary microfluidic chip with an inner phase outlet diameter of 200 mu m and an outer phase inner diameter of 1mm is adopted, spinning solution is used as an inner phase, ethanol is used as an outer phase, and the inner phase flow rate is controlled to be 5mL/h and the outer phase flow rate is controlled to be 50mL/h through a digital microfluidic control pump. And adjusting the included angle between the microfluidic chip and the horizontal plane to be 90 degrees, collecting the obtained spiral fiber through a winding device, and carrying out appearance and performance tests. The optical micrograph of the obtained spiral fiber is shown in FIG. 7, and it can be seen that the diameter of the spiral fiber was 68 μm, the pitch was 595 μm, and the amplitude was 189 μm. Tensile strength results are shown in Table 1 below, from which it can be seen that the resulting helical fiber has a tensile strength of 12 MPa.
TABLE 1 spiral fiber morphology and Strength
Claims (8)
1. A micro-fluidic spinning construction method of high-strength spiral fibers comprises the following specific steps:
A. dissolving a polymer in a solvent to prepare a uniform solution to obtain a spinning solution;
B. adopting a coaxial capillary microfluidic chip, taking the spinning solution obtained in the step A as an inner phase, taking a coagulant as an outer phase, and controlling the flow velocity of the inner phase and the flow velocity of the outer phase through a microfluidic pump to carry out microfluidic spinning;
C. and C, adjusting an included angle between the microfluidic chip and the horizontal plane, and collecting the spiral fiber obtained in the step B through a winding device.
2. The method according to claim 1, wherein the polymer material in step A is polycaprolactone, polyurethane, polyvinyl butyral, polysulfone, polyethersulfone, or polyvinyl alcohol.
3. The microfluidic spinning building method according to claim 1, wherein the solvent in step a is at least one of formic acid, dichloromethane, N-dimethylformamide, dimethylsulfoxide or ethanol.
4. The microfluidic spinning building method according to claim 1, wherein the mass concentration of the spinning solution in step a is 10-25%.
5. The microfluidic spinning construction method as claimed in claim 1, wherein the diameter of the phase outlet in the coaxial capillary microfluidic chip in step B is 100-200 μm.
6. The microfluidic spinning building method according to claim 1, wherein the coagulant in step B is at least one of water, methanol, ethanol, dimethyl sulfoxide, and N, N-dimethylformamide.
7. The microfluidic spinning building method according to claim 1, wherein the flow rate of the inner phase in step B is 1-5 mL/h, and the flow rate of the outer phase is 10-50 mL/h.
8. The microfluidic spinning construction method according to claim 1, wherein an included angle between the microfluidic chip in the step C and a horizontal plane is 0-90 °.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114836845A (en) * | 2022-05-20 | 2022-08-02 | 武汉纺织大学 | Flexible conductive polyurethane fiber and preparation method thereof |
| CN114875661A (en) * | 2022-05-27 | 2022-08-09 | 中钢集团南京新材料研究院有限公司 | Flexible magnetoelectric fiber with force-electricity conversion effect, manufacturing method thereof and related product |
| CN115012055A (en) * | 2022-05-27 | 2022-09-06 | 中钢集团南京新材料研究院有限公司 | Preparation method of flexible stretchable magnetic wire and flexible stretchable magnetic wire |
| CN116971059A (en) * | 2023-08-18 | 2023-10-31 | 北京服装学院 | Composite hydrogel fiber and preparation method and application thereof |
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| CN114836845A (en) * | 2022-05-20 | 2022-08-02 | 武汉纺织大学 | Flexible conductive polyurethane fiber and preparation method thereof |
| CN114836845B (en) * | 2022-05-20 | 2023-08-25 | 武汉纺织大学 | Flexible conductive polyurethane fiber and preparation method thereof |
| CN114875661A (en) * | 2022-05-27 | 2022-08-09 | 中钢集团南京新材料研究院有限公司 | Flexible magnetoelectric fiber with force-electricity conversion effect, manufacturing method thereof and related product |
| CN115012055A (en) * | 2022-05-27 | 2022-09-06 | 中钢集团南京新材料研究院有限公司 | Preparation method of flexible stretchable magnetic wire and flexible stretchable magnetic wire |
| CN116971059A (en) * | 2023-08-18 | 2023-10-31 | 北京服装学院 | Composite hydrogel fiber and preparation method and application thereof |
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