CN109957852A - A kind of composite nano fiber electrostatic spinning process - Google Patents

A kind of composite nano fiber electrostatic spinning process Download PDF

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Publication number
CN109957852A
CN109957852A CN201910265156.5A CN201910265156A CN109957852A CN 109957852 A CN109957852 A CN 109957852A CN 201910265156 A CN201910265156 A CN 201910265156A CN 109957852 A CN109957852 A CN 109957852A
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CN
China
Prior art keywords
electrostatic spinning
spinning
fibre
forming polymer
subjected
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Pending
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CN201910265156.5A
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Chinese (zh)
Inventor
柯惠珍
李永贵
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Minjiang University
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Minjiang University
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Priority to CN201910265156.5A priority Critical patent/CN109957852A/en
Publication of CN109957852A publication Critical patent/CN109957852A/en
Pending legal-status Critical Current

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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0015Electro-spinning characterised by the initial state of the material
    • D01D5/003Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/02Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/08Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyacrylonitrile as constituent

Abstract

The invention discloses a kind of composite nano fiber electrostatic spinning process, comprise the following steps that S1, fibre-forming polymer is carried out sorting break process;S2, the broken rear fibre-forming polymer of step S1 is subjected to decolorization by hydrogen peroxide;S3, fibre-forming polymer after step S2 decoloration is subjected to washing process, be washed with deionized water completely, moisture removal is removed in drying;S4, fibre-forming polymer is subjected to dissolution process;S5, spinning is carried out to solution using electrostatic spinning technique, obtain nanofiber, beneficial effects of the present invention are as follows: the technique is using conventional electrostatic spinning, raw material can be made using waste and old fibrous material, mixing electrostatic spinning liquid can be produced by simple processing step, can relatively easily prepare the lower composite nano fiber product of diameter, relatively simple solvent and separation method can be adapted for multiple polymers nanofiber, raw material is cheap and easy to get, low in cost, environmentally protective.

Description

A kind of composite nano fiber electrostatic spinning process
Technical field
The invention discloses a kind of composite nano fiber electrostatic spinning process, belong to textile technology technical field.
Background technique
Electrostatic spinning technique refers to that polymer solution or melt occur injection under the effect of high-voltage electrostatic field power and stretch, through molten Agent volatilization or cooling and solidifying, obtain a kind of method of fibrous material.Electrostatic spinning is most main relative to other conventional spinning processes The characteristics of wanting is that the nanofiber that large specific surface area, porosity are high, aperture is small, draw ratio is big can be obtained, in cell culture, environment There is significant meaning in the fields such as protection and improvement.
Summary of the invention
The purpose of the invention is to provide a kind of composite nano fiber electrostatic spinning process.
To achieve the above object, the invention provides the following technical scheme: a kind of composite nano fiber electrostatic spinning process, packet Include that steps are as follows:
S1, fibre-forming polymer is subjected to sorting break process;
S2, the broken rear fibre-forming polymer of step S1 is subjected to decolorization by hydrogen peroxide;
S3, fibre-forming polymer after step S2 decoloration is subjected to washing process, be washed with deionized water completely, drying goes to remove water Point;
S4, fibre-forming polymer is subjected to dissolution process:
A, polyacrylonitrile and n,N-Dimethylformamide are placed in container, are stirred under room temperature completely molten to polyacrylonitrile Solution obtains polyacrylonitrile solution in n,N-Dimethylformamide;
B, acetylbutyrylcellulose and n,N-Dimethylformamide and acetone are placed in container, are stirred under room temperature to vinegar Sour cellulose butyrate is completely dissolved, and obtains acetylbutyrylcellulose solution;
C, it weighs polyacrylonitrile solution and acetylbutyrylcellulose solution is placed in container, mixed after being stirred under room temperature Electrostatic spinning liquid;
S5, spinning is carried out to solution using electrostatic spinning technique, obtains composite nano fiber:
D, mixing electrostatic spinning liquid is fitted into the syringe that volume is 10mL, and spinning syringe needle uses No. 21 stainless steel syringe needles, For precise injection pump control spinning speed in 1.5mL/h, high voltage power supply controls voltage in 15kV, air compressor control auxiliary gas Pressure in 80~200kpa;
E, spinning is carried out in the reception device of electrostatic spinning, prepares disorderly arranged nanofiber.
Preferably, the concentration for mixing electrostatic spinning liquid in the step S4 is 12%~15%.
Preferably, regulating environmental humidity is 20~50% in the step S5, temperature is 20~50 DEG C, in spinning syringe needle Diameter is 0.2~2mm, and receiving distance is 10~20cm.
Preferably, the hydrogen peroxide concentration in the step S2 is 20-30%.
Compared with prior art, beneficial effects of the present invention are as follows:
In the present invention, which can make raw material using waste and old fibrous material, by simple using conventional electrostatic spinning Processing step can produce mixing electrostatic spinning liquid, can relatively easily prepare the lower nanofiber product of diameter, compared with It can be adapted for multiple polymers nanofiber for simple solvent and separation method, raw material is cheap and easy to get, low in cost, green Environmental protection.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
Embodiment one
A kind of composite nano fiber electrostatic spinning process, comprises the following steps that
S1, fibre-forming polymer is subjected to sorting break process;
S2, the broken rear fibre-forming polymer of step S1 is subjected to decolorization by hydrogen peroxide;
S3, fibre-forming polymer after step S2 decoloration is subjected to washing process, be washed with deionized water completely, drying goes to remove water Point;
S4, fibre-forming polymer is subjected to dissolution process:
A, polyacrylonitrile and n,N-Dimethylformamide are placed in container, are stirred under room temperature completely molten to polyacrylonitrile Solution obtains polyacrylonitrile solution in n,N-Dimethylformamide;
B, acetylbutyrylcellulose and n,N-Dimethylformamide and acetone are placed in container, are stirred under room temperature to vinegar Sour cellulose butyrate is completely dissolved, and obtains acetylbutyrylcellulose solution;
C, it weighs polyacrylonitrile solution and acetylbutyrylcellulose solution is placed in container, mixed after being stirred under room temperature Electrostatic spinning liquid;
S5, spinning is carried out to solution using electrostatic spinning technique, obtains nanofiber:
D, mixing electrostatic spinning liquid is fitted into the syringe that volume is 10mL, and spinning syringe needle uses No. 21 stainless steel syringe needles, For precise injection pump control spinning speed in 1.5mL/h, high voltage power supply controls voltage in 15kV, air compressor control auxiliary gas Pressure in 80kpa;
E, spinning is carried out in the reception device of electrostatic spinning, prepares disorderly arranged nanofiber, and spinning process is suitable Freely, gained fiber is continuous, and surface is smooth, and it is few between fiber be adhered, have preferable spinnability.
Wherein, the concentration that electrostatic spinning liquid is mixed in the step S4 is 12%.
Wherein, regulating environmental humidity is 20% in the step S5, and temperature is 20 DEG C, and spinning syringe needle internal diameter is 0.2mm, is connect Receiving distance is 10cm.
Wherein, the hydrogen peroxide concentration in the step S2 is 20%.
Embodiment two
A kind of composite nano fiber electrostatic spinning process, comprises the following steps that
S1, fibre-forming polymer is subjected to sorting break process;
S2, the broken rear fibre-forming polymer of step S1 is subjected to decolorization by hydrogen peroxide;
S3, fibre-forming polymer after step S2 decoloration is subjected to washing process, be washed with deionized water completely, drying goes to remove water Point;
S4, fibre-forming polymer is subjected to dissolution process:
A, polyacrylonitrile and n,N-Dimethylformamide are placed in container, are stirred under room temperature completely molten to polyacrylonitrile Solution obtains polyacrylonitrile solution in n,N-Dimethylformamide;
B, acetylbutyrylcellulose and n,N-Dimethylformamide and acetone are placed in container, are stirred under room temperature to vinegar Sour cellulose butyrate is completely dissolved, and obtains acetylbutyrylcellulose solution;
C, it weighs polyacrylonitrile solution and acetylbutyrylcellulose solution is placed in container, mixed after being stirred under room temperature Electrostatic spinning liquid;
S5, spinning is carried out to solution using electrostatic spinning technique, obtains nanofiber:
D, mixing electrostatic spinning liquid is fitted into the syringe that volume is 10mL, and spinning syringe needle uses No. 21 stainless steel syringe needles, For precise injection pump control spinning speed in 1.5mL/h, high voltage power supply controls voltage in 15kV, air compressor control auxiliary gas Pressure in 200kpa;
E, spinning is carried out in the reception device of electrostatic spinning, prepares disorderly arranged nanofiber, and spinning process is suitable Freely, gained fiber is continuous, and surface is smooth, and it is few between fiber be adhered, have preferable spinnability.
Wherein, the concentration that electrostatic spinning liquid is mixed in the step S4 is 15%.
Wherein, regulating environmental humidity is 50% in the step S5, and temperature is 50 DEG C, and spinning syringe needle internal diameter is 0.2mm, is connect Receiving distance is 20cm.
Wherein, the hydrogen peroxide concentration in the step S2 is 30%.
Embodiment three
A kind of composite nano fiber electrostatic spinning process, comprises the following steps that
S1, fibre-forming polymer is subjected to sorting break process;
S2, the broken rear fibre-forming polymer of step S1 is subjected to decolorization by hydrogen peroxide;
S3, fibre-forming polymer after step S2 decoloration is subjected to washing process, washed with clean water, moisture removal is removed in drying;
S4, fibre-forming polymer is subjected to dissolution process:
A, polyacrylonitrile and n,N-Dimethylformamide are placed in container, are stirred under room temperature completely molten to polyacrylonitrile Solution obtains polyacrylonitrile solution in n,N-Dimethylformamide;
B, acetylbutyrylcellulose and n,N-Dimethylformamide and acetone are placed in container, are stirred under room temperature to vinegar Sour cellulose butyrate is completely dissolved, and obtains acetylbutyrylcellulose solution;
C, it weighs polyacrylonitrile solution and acetylbutyrylcellulose solution is placed in container, mixed after being stirred under room temperature Electrostatic spinning liquid;
S5, spinning is carried out to solution using electrostatic spinning technique, obtains nanofiber:
D, mixing electrostatic spinning liquid is fitted into the syringe that volume is 10mL, and spinning syringe needle uses No. 21 stainless steel syringe needles, For precise injection pump control spinning speed in 1.5mL/h, high voltage power supply controls voltage in 15kV, air compressor control auxiliary gas Pressure in 150kpa;
E, spinning is carried out in the reception device of electrostatic spinning, prepares disorderly arranged nanofiber, and gained fiber connects Continuous, surface is smooth, and it is few between fiber be adhered, there is preferable spinnability.
Wherein, the concentration that electrostatic spinning liquid is mixed in the step S4 is 14%.
Wherein, regulating environmental humidity is 35% in the step S5, and temperature is 35 DEG C, and spinning syringe needle internal diameter is 1.5mm, is connect Receiving distance is 15cm.
Wherein, the hydrogen peroxide concentration in the step S2 is 25%.
Beneficial effects of the present invention are as follows: the technique can be made using conventional electrostatic spinning using waste and old fibrous material Raw material can produce mixing electrostatic spinning liquid by simple processing step, and it is lower multiple can relatively easily to prepare diameter Nanofiber product is closed, relatively simple solvent and separation method can be adapted for multiple polymers nanofiber, and raw material is cheap It is easy to get, it is low in cost, it is environmentally protective.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (4)

1. a kind of composite nano fiber electrostatic spinning process, which is characterized in that comprise the following steps that
S1, fibre-forming polymer is subjected to sorting break process;
S2, the broken rear fibre-forming polymer of step S1 is subjected to decolorization by hydrogen peroxide;
S3, fibre-forming polymer after step S2 decoloration is subjected to washing process, be washed with deionized water completely, moisture removal is removed in drying;
S4, fibre-forming polymer is subjected to dissolution process:
A, polyacrylonitrile and n,N-Dimethylformamide are placed in container, stirring to polyacrylonitrile is dissolved completely under room temperature In n,N-Dimethylformamide, polyacrylonitrile solution is obtained;
B, acetylbutyrylcellulose and n,N-Dimethylformamide and acetone are placed in container, are stirred under room temperature to acetic acid fourth Acid cellulose is completely dissolved, and obtains acetylbutyrylcellulose solution;
C, it weighs polyacrylonitrile solution and acetylbutyrylcellulose solution is placed in container, mixing electrostatic is obtained after stirring under room temperature Spinning solution;
S5, spinning is carried out to solution using electrostatic spinning technique, obtains nanofiber:
D, mixing electrostatic spinning liquid is fitted into the syringe that volume is 10mL, and spinning syringe needle uses No. 21 stainless steel syringe needles, accurate Syringe pump controls spinning speed in 1.5mL/h, and high voltage power supply controls voltage in 15kV, the pressure of air compressor control auxiliary gas In 80~200kpa;
E, spinning is carried out in the reception device of electrostatic spinning, prepares disorderly arranged nanofiber.
2. a kind of composite nano fiber electrostatic spinning process according to claim 1, it is characterised in that: in the step S4 The concentration for mixing electrostatic spinning liquid is 12%~15%.
3. a kind of composite nano fiber electrostatic spinning process according to claim 1, it is characterised in that: in the step S5 Regulating environmental humidity is 20~50%, and temperature is 20~50 DEG C, and spinning syringe needle internal diameter is 0.2~2mm, receive distance for 10~ 20cm。
4. a kind of composite nano fiber electrostatic spinning process according to claim 1, it is characterised in that: in the step S2 Hydrogen peroxide concentration be 20-30%.
CN201910265156.5A 2019-04-03 2019-04-03 A kind of composite nano fiber electrostatic spinning process Pending CN109957852A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114349871A (en) * 2022-01-11 2022-04-15 万华化学集团股份有限公司 Method for decoloring and decontaminating cellulose acetate butyrate
CN115385442A (en) * 2022-05-25 2022-11-25 天津大学 Composite functional micro-nano fiber carrier and preparation method and application thereof

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US4357389A (en) * 1979-09-10 1982-11-02 Asahi Kasei Kogyo Kabushiki Kaisha Polymer dope composition, composite fibers made therefrom and process for making same
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CN108149339A (en) * 2018-01-24 2018-06-12 湖州科博信息科技有限公司 A kind of recycling terylene nanometer Electrostatic spinning of fibres liquid
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Publication number Priority date Publication date Assignee Title
US4357389A (en) * 1979-09-10 1982-11-02 Asahi Kasei Kogyo Kabushiki Kaisha Polymer dope composition, composite fibers made therefrom and process for making same
CN101270198A (en) * 2008-05-15 2008-09-24 东华大学 Method for electrostatic blending polyacrylonitrile/glycol cellulose nano-fibrous membrane
CN106978647A (en) * 2017-04-26 2017-07-25 四川大学 A kind of production technology of nanofiber
CN108149339A (en) * 2018-01-24 2018-06-12 湖州科博信息科技有限公司 A kind of recycling terylene nanometer Electrostatic spinning of fibres liquid
CN108360144A (en) * 2018-01-24 2018-08-03 湖州科博信息科技有限公司 A kind of waste and old terylene textile recycling processing method

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114349871A (en) * 2022-01-11 2022-04-15 万华化学集团股份有限公司 Method for decoloring and decontaminating cellulose acetate butyrate
CN114349871B (en) * 2022-01-11 2022-11-08 万华化学集团股份有限公司 Method for decoloring and decontaminating cellulose acetate butyrate
CN115385442A (en) * 2022-05-25 2022-11-25 天津大学 Composite functional micro-nano fiber carrier and preparation method and application thereof
CN115385442B (en) * 2022-05-25 2023-07-04 天津大学 Composite functional micro-nanofiber carrier and preparation method and application thereof

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Application publication date: 20190702

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