CN108384574A - Compound desulfurizing film of a kind of electrostatic spinning biology and preparation method thereof - Google Patents
Compound desulfurizing film of a kind of electrostatic spinning biology and preparation method thereof Download PDFInfo
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- CN108384574A CN108384574A CN201810181273.9A CN201810181273A CN108384574A CN 108384574 A CN108384574 A CN 108384574A CN 201810181273 A CN201810181273 A CN 201810181273A CN 108384574 A CN108384574 A CN 108384574A
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- shell
- electrostatic spinning
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- film
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G31/00—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for
-
- 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
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- 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
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
-
- 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
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
Abstract
The invention discloses compound desulfurizing films of a kind of electrostatic spinning biology and preparation method thereof.The desulfurizing film is accumulated by several Random fibers, every fiber is made of stratum nucleare and shell, and shell includes the outer shell of hypostracum and package hypostracum, and stratum nucleare is the glycerine composition for being dispersed with desulfurization bacterium, hypostracum is polymer material layer, and outer shell is that 8 particle packings of several ZIF form.The preparation method is：Macromolecule dissolution is obtained to coaxial electrically spun shell liquid in organic solvent；2) bacterium is scattered in acquisition coaxial electrically spun core liquid in glycerine；3) shell core solution progress electrostatic spinning is obtained into static spinning membrane using electrospinning syringe needle；4) static spinning membrane is submerged initially in methylimidazole solution, adds zinc acetate solution, slight concussion, which is uniformly mixed, places several minutes；5) film that step 4) obtains is cleaned for several times with deionized water.The compound desulfurizing film of biology prepared by the present invention, process is easy, easy industrial mass production, has comparable desulphurizing activated and superior cyclical stability.
Description
Technical field
The invention belongs to Biocomposite material FIELD OF THE INVENTIONThe more particularly to a kind of electrostatic spinning compound desulfurizing film of biology and its
Preparation method.
Background technology
In the oil industry, sulfur-containing compound causes significant damage to human health and environmental protection.Biological desulfurization
It is acknowledged as a kind of effective sulfur method of green at present, immobilized that biological desulfurization is promoted to commercial Application is great using bacterium
Potentiality.There are three disadvantages for the immobilized tool of common bacterium：First, bacterium is low with carrier material combination degree, bacterium is easy to fall off；Second is that
Support material intensity is relatively low, and bacterium easily leakage is in external environment；Third, bacterium can not be evenly dispersed, active area is caused to reduce,
Mass transfer efficiency is low.Therefore it provides a kind of method that feasible effective immobilized bacterium carries out desulfurization be there is an urgent need to.
Invention content
Technical problem to be solved by the invention is to provide a kind of good compound desulfurizing films of electrostatic spinning biology of desulfurization effect
And preparation method thereof.
The technical solution taken by the invention to solve the above technical problem is：
A kind of compound desulfurizing film of electrostatic spinning biology, the compound desulfurizing film of the electrostatic spinning biology is by several Random fiber heaps
Product forms, and every fiber is made of stratum nucleare and shell, and the shell includes the outer shell of hypostracum and package hypostracum, the core
Layer is the glycerine composition for being dispersed with desulfurization bacterium, and the hypostracum is polymer material layer, and the outer shell is several ZIF-8 particles
It accumulates.
In said program, the polymer material layer is polycaprolactone layer.
In said program, the desulfurization bacterium is Gordonia amicalis WQ-01.
In said program, the technological parameter of electrostatic spinning is in step 3)：Receive distance 13-15cm；Receiver board voltage is set
It is set to 0 to -0.2kv；Voltage is set as 10-12kv at syringe needle；Inner core fltting speed is 0.1-0.15mm/min；Shell promotes speed
Degree is 7.0-8.0mm/min, spinning time 30-60min.
A kind of preparation method of the compound desulfurizing film of electrostatic spinning biology, includes the following steps：
1) high molecular material is dissolved in organic solvent, stirs to clarify bubble-free, obtain coaxial electrically spun shell liquid；
2) bacterium is cleaned with buffer solution and is scattered in afterwards in glycerine for several times, stirring at low speed makes bacterium be uniformly dispersed, and obtains
Coaxial electrically spun core liquid；
3) shell core solution is subjected to electrostatic spinning using electrospinning syringe needle, obtains static spinning membrane；
4) static spinning membrane is submerged initially in methylimidazole solution, adds zinc acetate solution, slight concussion is uniformly mixed
It places；
5) film that step 4) obtains is cleaned with deionized water.
In said program, the organic solvent is chloroform.
In said program, the organic solvent further includes the dimethylformamide that mass fraction is 0-15%.
In said program, the high molecular material is polycaprolactone.
In said program, the high molecular material further includes the polyethylene glycol that mass fraction is 0-10%.
In said program, the desulfurization bacterium is Gordonia amicalis WQ-01.
In said program, the technological parameter of electrostatic spinning is in step 3)：Receive distance 13-15cm；Receiver board voltage is set
It is set to 0 to -0.2kv；Voltage is set as 10-12kv at syringe needle；Inner core fltting speed is 0.1-0.15mm/min；Shell promotes speed
Degree is 7.0-8.0mm/min, spinning time 30-60min.
The compound desulfurizing film of biology being made using the immobilized desulfurizing bacteria of coaxial electrostatic spinning technology the present invention provides a kind of
Method.First by macromolecule dissolution in organic solvent, bubble-free is stirred to clarify, coaxial electrically spun shell liquid is obtained, bacterium is used
PBS solution cleaning is scattered in glycerine afterwards for several times, and stirring at low speed makes bacterium be uniformly dispersed, and obtains coaxial electrically spun core liquid；By same
Axis electrostatic spinning obtains biological desulphurization composite membrane, finally continuous fine and close in one layer of coaxial electrostatic spinning fiber surface growth in situ
ZIF-8 shells.
Beneficial effects of the present invention are as follows：The maximum innovation of the present invention is to synthesize a kind of fibre by coaxial electrostatic spinning technology
Hollow membrane structure is tieed up, to be provided certain living space by immobilized bacterium so that bacterium while immobilized again have compared with
High bioactivity, and increase the adsorption rate that material hydrophobic improves sulphur-containing substance at ZIF-8 shells in fibrous appearance.This
Kind method is easy with process, easy industrial mass production, by the way that bacterium is immobilized in coaxial electrostatic spinning tunica fibrosa, utilization
The larger specific surface area of electrostatic spinning enables bacterium efficiently to be exchanged with external substance, and relatively independent space is but also production
There is the biological composite membrane gone out comparable desulphurizing activated, larger hydrophobicity to be combined absorption desulfurization with biological desulphurization, make simultaneously
At film can effectively improve the cyclical stability of bacterium.
Description of the drawings
Fig. 1 is the structural schematic diagram of the compound desulfurizing film of electrostatic spinning biology of 1 gained of embodiment.
Fig. 2 is the photo of the compound desulfurizing film of electrostatic spinning biology of 1 gained of embodiment.
Fig. 3 is the stereoscan photograph of the compound desulfurizing film of electrostatic spinning biology of 1 gained of embodiment：A) unmodified low amplification
Multiple, b) unmodified high-amplification-factor, c) unmodified section, d) after modification ZIF-8.
Fig. 4 is the fluorescent microscopy images of the compound desulfurizing film of electrostatic spinning biology of 1 gained of embodiment：A) visible light shines
Piece, b) fluorescence photo.
Fig. 5 is the contact angle of the compound desulfurizing film of electrostatic spinning biology of 1 gained of embodiment：A) unmodified, b) modification ZIF-8
Afterwards.
Fig. 6 is the catalytic performance test of electrostatic spinning the biology compound desulfurizing film and naked bacterium of 1 gained of embodiment
Fig. 7 is that the compound desulfurizing film of electrostatic spinning biology of 1 gained of embodiment and the cycle performance of naked bacterium are tested.
Specific implementation mode
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment 1
As shown in Figure 1, it is a kind of compound desulfurizing film of electrostatic spinning biology provided in this embodiment, the electrostatic spinning life
The compound desulfurizing film of object is accumulated by several Random fibers, and every fiber is made of stratum nucleare and shell, shell include hypostracum and
The outer shell of hypostracum is wrapped up, stratum nucleare is the glycerine composition for being dispersed with desulfurizing bacteria, and hypostracum is polymer material layer, outer shell
It is formed for several ZIF-8 particle packings.In the present embodiment, high molecular material is polycaprolactone.Desulfurizing bacteria is Gordonia
Amicalis WQ-01, derive from Chinese industrial Microbiological Culture Collection administrative center, and deposit number is CICC 20663.
The present embodiment also provides a kind of method preparing the compound desulfurizing film of the biology using coaxial electrostatic spinning, specific to grasp
Steps are as follows for work：
(1) it is 9 2g polycaprolactones to be dissolved in 20g mass ratioes：In 1 chloroform and the mixed solution of dimethylformamide,
It stirs to clarify, is protected from light and stands to no bubble, it is for use as electrospinning external solution；
(2) 5ml is taken to be cleaned with PBS solution the friendly Gordonia bronchialis Gordonia amicalis WQ-01 that OD values are 1.0
It concentrates, is scattered in 2ml glycerine for several times, stirring at low speed is for use as liquid in electrospinning to being uniformly dispersed；
(3) coaxial electrostatic spinning is assembled, interior external solution is used respectively 5ml syringes be mounted on and promotes on pump；
(4) it receiving distance and is set as 14cm, receiver board voltage is set as -0.15kv, and voltage is set as 10.5kv at syringe needle,
Inner core fltting speed is 0.1165mm/min, and shell fltting speed is 0.7000mm/min, and spinning carries out 30min, in receiver board
Obtain static spinning membrane；
(5) static spinning membrane obtained is cut into 5cm × 5cm, after cleaning one time with deionized water, immerses the two of 5ml
In methyl imidazole solution (160mM), then the zinc acetate solution (40mM) of addition 5ml is spent after slightly shaking 5min into solution
Ionized water cleans one time again.
Embodiment 2
The present embodiment provides a kind of method preparing the compound desulfurizing film of the biology using coaxial electrostatic spinning, concrete operations
Steps are as follows：
(1) 2g polycaprolactones are dissolved in chloroform, are stirred to clarify, be protected from light standing to no bubble, as electrospinning outside
Liquid is for use；
(2) 5ml is taken to be cleaned with PBS solution the friendly Gordonia bronchialis Gordonia amicalis WQ-01 that OD values are 1.0
It concentrates, is scattered in 2ml glycerine for several times, stirring at low speed is for use as liquid in electrospinning to being uniformly dispersed；
(3) coaxial electrostatic spinning is assembled, interior external solution is used respectively 5ml syringes be mounted on and promotes on pump；
(4) it receiving distance and is set as 14cm, receiver board voltage is set as -0.15kv, and voltage is set as 10.5kv at syringe needle,
Inner core fltting speed is 0.1165mm/min, and shell fltting speed is 0.7000mm/min, and spinning carries out 30min, in receiver board
Obtain static spinning membrane.
(5) static spinning membrane obtained is cut into 5cm × 5cm, after cleaning one time with deionized water, immerses the two of 5ml
In methyl imidazole solution (160mM), then the zinc acetate solution (40mM) of addition 5ml is spent after slightly shaking 5min into solution
Ionized water cleans one time again.
Embodiment 3
The present embodiment provides a kind of method preparing the compound desulfurizing film of the biology using coaxial electrostatic spinning, concrete operations
Steps are as follows：
(1) it is 9 1.8g polycaprolactones and 0.2g polyethylene glycol to be dissolved in 20g mass ratioes：1 chloroform and dimethyl formyl
It in the mixed solution of amine, stirs to clarify, is protected from light and stands to no bubble, it is for use as electrospinning external solution；
(2) 5ml is taken to be cleaned with PBS solution the friendly Gordonia bronchialis Gordonia amicalis WQ-01 that OD values are 1.0
It concentrates, is scattered in 2ml glycerine for several times, stirring at low speed is for use as liquid in electrospinning to being uniformly dispersed；
(3) coaxial electrostatic spinning is assembled, interior external solution is used respectively 5ml syringes be mounted on and promotes on pump；
(4) it receiving distance and is set as 14cm, receiver board voltage is set as -0.15kv, and voltage is set as 10.5kv at syringe needle,
Inner core fltting speed is 0.1165mm/min, and shell fltting speed is 0.7000mm/min, and spinning carries out 30min, in receiver board
Obtain static spinning membrane.
(5) static spinning membrane obtained is cut into 5cm × 5cm, after cleaning one time with deionized water, invades the two of 5ml
In methyl imidazole solution (160mM), then the zinc acetate solution (40mM) of addition 5ml is spent after slightly shaking 5min into solution
Ionized water cleans one time again.
As shown in Fig. 2, the membrane structure for the electrostatic spinning biological composite membrane being prepared is complete, there is comparable mechanical property
Energy.As shown in figure 3, the electrostatic spinning biological composite membrane prepared is showed under a scanning electron microscope by 3 microns of diameter
Fiber accumulations form, it is meant that very high specific surface area, according to section as can be seen that fiber be nucleocapsid, by Fig. 3 d
It can be seen that the fibrous outer after modification has the continuous ZIF-8 particles of one layer of densification, particle diameter is in 100nm or so.Fig. 4 a
It as can be seen that electrospinning fibre is nucleocapsid, can be seen that bacterium is scattered in the core arrangement of fiber by Fig. 4 b, demonstrate thin
Born of the same parents are by immobilized in relatively independent doughnut.Fig. 5 is the contact angle of spinning film and spinning film after modification ZIF-8, Ke Yiguan
It observes unmodified contact angle and is less than 90 degree, do not have hydrophobicity, and the film contact angle after modifying has higher at 123 degree
Hydrophobicity has good adsorption effect to oil phase.Fig. 6 is that bacterium carries out desulfurization performance test with spinning film, can be observed
The naked bacterium catalytic rate highest in 40h, unmodified biological composite membrane just reach higher catalytic efficiency in 80h or so, and
Biological composite membrane after modification ZIF-8 just surpasses in reverse the catalytic efficiency of naked bacterium in 50h or so, illustrates because beam is not present in protoblast
Effect is tied up, is showing higher catalytic efficiency in early days, always above unmodified biological composite membrane, but because of the life after modification
There is object composite membrane physically better suction-operated to show higher catalytic efficiency.It is surveyed as seen from Figure 7 in cyclicity
In examination experiment, protoblast is after cycle 5 times, and relative activity has already decreased to 35%, and unmodified and modification ZIF-8 biology is multiple
Film is closed after loop test 5 times, relative activity is kept at 73% and 82%, it is seen that unmodified and modified biology is compound
The stability of film is far above the stability of naked bacterium, and the biomembrane of modified ZIF-8 is led due to the presence of shell decorative material
The stability higher for causing structure has better stability, the cycle of such biological composite membrane compared to unmodified biomembrane
Stability means its possessed superelevation potentiality in commercial Application.
Obviously, above-described embodiment is only intended to clearly illustrate example made by the present invention, and not to embodiment
Limitation.For those of ordinary skill in the art, other different forms can also be made on the basis of the above description
Variation or variation.There is no necessity and possibility to exhaust all the enbodiments.And it is therefore amplified obvious
Variation changes within still in the protection domain of the invention.
Claims (10)
1. a kind of compound desulfurizing film of electrostatic spinning biology, which is characterized in that the compound desulfurizing film of the electrostatic spinning biology is by several
Random fiber is accumulated, and every fiber is made of stratum nucleare and shell, and the shell includes the outer of hypostracum and package hypostracum
Shell, the stratum nucleare are the glycerine composition for being dispersed with desulfurization bacterium, and the hypostracum is polymer material layer, if the outer shell is
Dry ZIF-8 particle packings form.
2. the compound desulfurizing film of electrostatic spinning biology as described in claim 1, which is characterized in that the polymer material layer is poly-
Caprolactone layer.
3. the compound desulfurizing film of electrostatic spinning as described in claim 1 biology, which is characterized in that the desulfurization bacterium is
Gordoniaamicalis WQ-01。
4. a kind of preparation method of the compound desulfurizing film of electrostatic spinning biology, which is characterized in that include the following steps：
1) high molecular material is dissolved in organic solvent, stirs to clarify bubble-free, obtain coaxial electrically spun shell liquid；
2) bacterium is cleaned with buffer solution and is scattered in afterwards in glycerine for several times, stirring at low speed makes bacterium be uniformly dispersed, and obtains coaxial
Electrospinning core liquid；
3) shell core solution is subjected to electrostatic spinning using electrospinning syringe needle, obtains static spinning membrane；
4) static spinning membrane is submerged initially in methylimidazole solution, adds zinc acetate solution, slight concussion, which is uniformly mixed, places；
5) film that step 4) obtains is cleaned with deionized water.
5. preparation method as claimed in claim 4, which is characterized in that the organic solvent is chloroform.
6. preparation method as claimed in claim 5, which is characterized in that the organic solvent further includes that mass fraction is 0-15%
Dimethylformamide.
7. preparation method as claimed in claim 4, which is characterized in that the high molecular material is polycaprolactone.
8. preparation method as claimed in claim 7, which is characterized in that the high molecular material further includes that mass fraction is 0-
10% polyethylene glycol.
9. preparation method as claimed in claim 4, which is characterized in that the desulfurization bacterium is Gordonia amicalis WQ-
01。
10. preparation method as claimed in claim 4, which is characterized in that the technological parameter of electrostatic spinning is in step 3)：It receives
Distance 13-15cm；Receiver board voltage is set as 0 to -0.2kv；Voltage is set as 10-12kv at syringe needle；Inner core fltting speed is
0.1-0.15mm/min；Shell fltting speed is 7.0-8.0mm/min, spinning time 30-60min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810181273.9A CN108384574B (en) | 2018-03-06 | 2018-03-06 | Electrostatic spinning biological composite desulphurization membrane and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810181273.9A CN108384574B (en) | 2018-03-06 | 2018-03-06 | Electrostatic spinning biological composite desulphurization membrane and preparation method thereof |
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| Publication Number | Publication Date |
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| CN108384574A true CN108384574A (en) | 2018-08-10 |
| CN108384574B CN108384574B (en) | 2020-04-21 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101705529A (en) * | 2009-10-29 | 2010-05-12 | 无锡中科光远生物材料有限公司 | Composite superfine fibre membrane of biologic compatible shell core structure and preparation method thereof |
| CN102733000A (en) * | 2012-06-27 | 2012-10-17 | 中国科学院过程工程研究所 | Preparation method for hollow polymer nanofibers |
| CN104651269A (en) * | 2015-01-06 | 2015-05-27 | 江南大学 | Desulphurizing bacterium for efficiently degrading DBT and application of desulphurizing bacterium in desulfurization |
| CN107051398A (en) * | 2017-04-26 | 2017-08-18 | 浙江大学 | A kind of method for preparing silk-fibroin nanofiber-metal organic frame laminated film |
-
2018
- 2018-03-06 CN CN201810181273.9A patent/CN108384574B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101705529A (en) * | 2009-10-29 | 2010-05-12 | 无锡中科光远生物材料有限公司 | Composite superfine fibre membrane of biologic compatible shell core structure and preparation method thereof |
| CN102733000A (en) * | 2012-06-27 | 2012-10-17 | 中国科学院过程工程研究所 | Preparation method for hollow polymer nanofibers |
| CN104651269A (en) * | 2015-01-06 | 2015-05-27 | 江南大学 | Desulphurizing bacterium for efficiently degrading DBT and application of desulphurizing bacterium in desulfurization |
| CN107051398A (en) * | 2017-04-26 | 2017-08-18 | 浙江大学 | A kind of method for preparing silk-fibroin nanofiber-metal organic frame laminated film |
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