CN108914375A - A kind of preparation method of long acting antibiotic polylactic acid fiber membrane - Google Patents
A kind of preparation method of long acting antibiotic polylactic acid fiber membrane Download PDFInfo
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- CN108914375A CN108914375A CN201811104017.6A CN201811104017A CN108914375A CN 108914375 A CN108914375 A CN 108914375A CN 201811104017 A CN201811104017 A CN 201811104017A CN 108914375 A CN108914375 A CN 108914375A
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- 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
- D04H1/4326—Condensation or reaction polymers
- D04H1/435—Polyesters
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- 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
- D04H1/413—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 containing granules other than absorbent substances
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- 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
Abstract
The invention discloses a kind of preparation methods of long acting antibiotic polylactic acid fiber membrane, belong to environment-friendly materials technical field.By polyethylene glycol and methylene chloride by volume 2：7~2：8 are mixed in blender, and 0.1~0.3 times of polyethylene glycol volume of antibacterial additives and 1.0~1.4 times of polyethylene glycol volume of polylactic acid are added to blender, in temperature be 40~50 DEG C, under conditions of revolving speed is 380~500r/min, after being stirred 30~60min, and 20~40min of ultrasonic disperse under conditions of frequency is 45~55kHz, obtain spinning solution, spinning solution is formed a film through electrostatic spinning to get long acting antibiotic polylactic acid fiber membrane.The long acting antibiotic polylactic acid fiber membrane of technical solution of the present invention preparation has the characteristics that excellent anti-microbial property and long acting antibiotic performance, has broad prospects in the development of environment-friendly materials technology industry.The ceramic grind additives of technical solution of the present invention preparation have the characteristics that excellent grinding aid efficiency, have broad prospects in the development of ceramic inorganic agent technology industry.
Description
Technical field
The invention discloses a kind of preparation methods of long acting antibiotic polylactic acid fiber membrane, belong to environment-friendly materials technical field.
Background technique
Acid fiber by polylactic be using the amyloid agricultural product such as corn, wheat, beet as raw material, after fermented generation lactic acid,
It is that a kind of raw material can be planted, easily be planted that acid fiber by polylactic, which is made, through polycondensation and melt spinning again, waste can in nature from
The synthetic fibers so degraded.It can be analyzed to carbon dioxide and water through microbial action in soil or seawater, will not when burning
Poison gas is distributed, will not be polluted, is a kind of ecological fiber of sustainable development.Its fabric feel, drapability are good, anti-purple
Outside line is suitable for various fashionable dresses, easy dress, sports goods and health and uses with lower flammable and excellent processing performance
Product etc., have broad application prospects.
The raw materials for production lactic acid of acid fiber by polylactic (PLA) is made from cornstarch, so being also known as this fiber
Zein fiber can be made with garden beet or cereal etc. through glucose fermentation, prepare the polymeric cost of lactic acid with reduction.Pass through cream
The polylactic acid of the available high molecular weight of direct polymerization of the chemical polymerization or lactic acid of sour Cyclodimerization object.Using polylactic acid as raw material
Obtained product has good biocompatibility and Bioabsorbable and biocidal property, anti-flammability, and degradable
In thermoplastic macromolecule material, PLA has best heat resistance.PLA fiber has same PET fiber (i.e. polyester fiber) similar
Physical characteristic not only has high crystalline, also has the same transparency；And due to its high crystalline and high-orientation,
To have high-fire resistance and high intensity, and it is not necessarily to special equipment and operating procedure, it can be into using conventional processing technology
Row spinning.It all joined a certain amount of antibacterial agent in artificial anti-bacterial fibre at present, the additional amount of antibacterial agent in the fibre is generally very
It is few, under the premise of not changing the traditional performance and processing performance of fiber, antibacterial agent is allowed to play sterilization or antibacterial effect.Existing rank
Antibacterial agent used in Duan Jiagong anti-bacterial fibre mainly has inorganic, organic and natural three categories.Wherein natural antibacterial agent and organic anti-
Microbial inoculum generally can make antibacterial agent adsorb or be bonded on textile fabric and obtain antibacterial by the methods of impregnating, padding and be grafted
Function, but the antibacterial effect and safety of natural antibacterial agent and organic antibacterial agent are unable to get guarantee, and inorganic antiseptic because with
The binding force of textile fabric is poor, between directly using the intertwined point for being only capable of being adsorbed on fiber surface or textile, just once washing
It is easy to fall off from fiber and reduce, even lose antibiotic property.
And traditional long acting antibiotic polylactic acid fiber membrane is there is also anti-microbial property is bad and the short problem of antibacterial timeliness, because
This, the shortcomings that how improving traditional long acting antibiotic polylactic acid fiber membrane, develops the length with good comprehensive performance in the hope of exploring
Imitating antibacterial polylactic acid fiber film is problem to be solved.
Summary of the invention
The present invention solves the technical problem of：For traditional long acting antibiotic polylactic acid fiber membrane anti-microbial property it is bad and
The short disadvantage of antibacterial timeliness provides a kind of preparation method of long acting antibiotic polylactic acid fiber membrane.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that：
A kind of preparation method of long acting antibiotic polylactic acid fiber membrane, specific preparation step are：
（1）Mixed-powder is calcined, is washed, it is dry, pretreatment powder is obtained, by pretreatment powder and water in mass ratio 1：10~1：
15 mixing, and the polyallylamine hydrochlorides of 0.3~0.6 times of powder quality of pretreatment are added, after ultrasonic disperse, obtain pretreatment powder
Mixture, by pretreatment mixture of powders and silver nitrate in mass ratio 10：3~10：4 mixing, after being stirred, filtering must change
Property powder；
（2）By modified powder and modified glucose solution in mass ratio 1：6~1：10 mixing, after being stirred to react, add modification
The sodium borohydride and 0.1~0.2 times of modified powder quality of trisodium citrate dihydrate that 0.1~0.2 times of powder quality, are stirred to react
Afterwards, it filters, obtains pretreatment antibacterial additives；
（3）By titanium source solution and sulfuric acid in mass ratio 1：4~1：6 mixing, and 1~2 times of titanium source quality of pretreatment addition is added
Agent after being stirred to react, after adjusting pH to 7.0~7.5, is aged, filters, wash, dry, obtains antibacterial additives；
（4）By polyethylene glycol and methylene chloride by volume 2：7~2：8 mixing, and it is added 0.1~0.3 times of polyethylene glycol volume
Antibacterial additives and 1.0~1.4 times of polyethylene glycol volume of polylactic acid, after being stirred, ultrasonic disperse obtains spinning solution, will
Spinning solution forms a film through electrostatic spinning to get long acting antibiotic polylactic acid fiber membrane.
Step（1）The mixed-powder is by titanium dioxide and potassium carbonate in molar ratio 4.0：1.3~4.0：1.5 mixing are ground
Mill, obtains mixed-powder.
Step（1）The calcination temperature is 750~850 DEG C.
Step（2）The modified glucose solution is by glucose and Potassiumiodate in mass ratio 1：2 mixing, and grape is added
The water that 20~30 times of saccharic amount after being stirred to react, is added 5~8 times of glucose quality of barium chloride solution, is stirred, filters,
Filtrate is obtained, by filtrate and metabisulfite solution in mass ratio 1：2 mixing, filtering, removal precipitating obtain modified glucose solution.
Step（3）The titanium source solution be the potassium fluotitanate solution that mass fraction is 10~15% or mass fraction be 8~
15% titanium tetrachloride solution.
Step（4）The polyethylene glycol is polyethylene glycol 400.
Step（4）The electrospinning conditions are 22 ± 2kV of spinning voltage, receive distance 12cm, fltting speed 1mL/
H, air humidity 10%, temperature are room temperature, and syringe needle internal diameter 0.6mm, uses aluminium foil as receiver used in spinning.
Step（4）The polylactic acid is the polylactic acid that molecular weight is 100000~120000.
The beneficial effects of the invention are as follows：
Antibacterial additives are added when preparing long acting antibiotic polylactic acid fiber membrane in the present invention in the product, firstly, antibacterial additives
The middle potassium tetratitanate for containing negative electrical charge using interlayer structure adsorbs silver ion, and polyallylamine salt is first used before adsorbing silver ion
Hydrochlorate pre-processes the lamellar structure of potassium tetratitanate, thus can be in polyallylamine hydrochlorides macromolecular when adsorbing silver ion
Silver ion uniform adsorption is improved into the antibacterial effect of antibacterial additives in the reunion in lamella, preventing silver ion under the action of chain,
And since after being added in product, potassium tetratitanate dispersibility preferably, and then improves the antibacterial effect of product, secondly, antibacterial
The polyallylamine hydrochlorides being added in additive can while being uniformly distributed silver ion, can in subsequent processes with change
Property glucose molecule chain formed microcapsules, and have pH responsiveness, microgel can be kept swollen while preparing cladding titanium dioxide
It is swollen, so that titanium dioxide is adsorbed in the pore structure after microgel expansion, and then improve titanium dioxide in antibacterial additives
Adsorbance, and improve in subsequent product preparation process the dispersibility of titanium dioxide, and then keep the antibiotic property of product further
It improves, furthermore, since the silver ion and titanium dioxide that are added in product can be by the lamella knots of the potassium tetratitanate in antibacterial additives
Structure protection, and be adsorbed in the microgel of piece interlayer, to make product that there is long-acting anti-microbial property.
Specific embodiment
By glucose and Potassiumiodate in mass ratio 1：2 are mixed in flask, and into flask be added glucose quality 20~
30 times of water, in temperature be 40~70 DEG C, under conditions of revolving speed is 300~380r/min, after being stirred to react 2~4h, then to burning
The mass fraction that 5~8 times of glucose quality are added in bottle is 20~25% barium chloride solutions, is 20~30 DEG C in temperature, revolving speed is
Under conditions of 250~350r/min, after being stirred 30~60min, filtering obtains filtrate, by filtrate and parts by weight be 20~
35% metabisulfite solution in mass ratio 1：2 mixing, in temperature be 20~30 DEG C, revolving speed be 250~350r/min under conditions of,
After being stirred 30~60min, filtering, removal precipitating obtains modified glucose solution；After mixed-powder is calcined 12~15h, obtain
Pre-process powder batch, powder batch will be pre-processed and first use mass fraction be 12~15% salt acid elution for 5~8 times after, then spend
Ion water washing 5~10 times, and by the pretreatment powder after washing be 80~90 DEG C in temperature under conditions of after dry 1~2h,
Powder must be pre-processed, by pretreatment powder and water in mass ratio 1：10~1：15 are mixed in beaker, and are added in advance into beaker
The polyallylamine hydrochlorides of 0.3~0.6 times of powder quality of processing, 1~2h of ultrasonic disperse under conditions of frequency is 45~55kHz
Afterwards, pretreatment mixture of powders is obtained, by pretreatment mixture of powders and silver nitrate in mass ratio 10：3~10：4 mixing, in temperature
It is 35~55 DEG C, after revolving speed is stirred 30~40min under conditions of being 300~400r/min, filtering obtains modified powder；It will
Modified powder and modified glucose solution in mass ratio 1：6~1：10 mixing, in temperature be 45~65 DEG C, revolving speed be 500~
Under conditions of 800r/min, after being stirred to react 1~2, then it is added and changes into modified powder and the mixture of modified glucose solution
0.1~0.2 times of powder quality of sodium borohydride of property and 0.1~0.2 times of modified powder quality of trisodium citrate dihydrate, in temperature
It is 60~75 DEG C, under conditions of revolving speed is 300~400r/min, after being stirred to react 2~3h, filtering must pre-process antibacterial addition
Agent；The sulfuric acid in mass ratio 1 for being 30~40% by titanium source solution and mass fraction：4~1：6 mixing, and to titanium source solution and sulfuric acid
Mixture in 1~2 times of titanium source quality of pretreatment additive is added, be 40~50 DEG C in temperature, revolving speed is 300~400r/
Under conditions of min, after being stirred to react 5~8h, antibacterial additives mixture is obtained, is adjusted with the ammonium hydroxide that mass fraction is 20~28%
After the pH to 7.0~7.5 of antibacterial additives mixture, after being aged 10~15h under room temperature, filtering obtains filter cake, by filter cake
After being washed with deionized 8~10 times, and 2~3h is dried under conditions of being 80~90 DEG C in temperature, obtains antibacterial additives；It will gather
Ethylene glycol and methylene chloride by volume 2：7~2：8 are mixed in blender, and polyethylene glycol volume is added into blender
0.1~0.3 times of antibacterial additives and 1.0~1.4 times of polyethylene glycol volume of polylactic acid, in temperature be 30~40 DEG C, revolving speed
Under conditions of 300~400r/min, after being stirred 1~2h, and the ultrasonic disperse 20 under conditions of frequency is 45~55kHz
~30min, obtains spinning solution, and spinning solution is formed a film through electrostatic spinning to get long acting antibiotic polylactic acid fiber membrane.The mixed-powder
For by titanium dioxide and potassium carbonate in molar ratio 4.0：1.3~4.0：1.5 mixed grindings, obtain mixed-powder.The calcination temperature
It is 750~850 DEG C.The titanium source solution is the potassium fluotitanate solution that mass fraction is 10~15% or mass fraction is 8~15%
Titanium tetrachloride solution.The polyethylene glycol is polyethylene glycol 400.The electrospinning conditions are 22 ± 2kV of spinning voltage, are connect
Distance 12cm is received, fltting speed 1mL/h, air humidity 10%, temperature is room temperature, syringe needle internal diameter 0.6mm used in spinning, is used
Aluminium foil is as receiver.The polylactic acid is the polylactic acid that molecular weight is 100000~120000.
By glucose and Potassiumiodate in mass ratio 1：2 are mixed in flask, and 30 times of glucose quality are added into flask
Water, in temperature be 70 DEG C, revolving speed be 380r/min under conditions of, after being stirred to react 4h, then into flask be added grape saccharic
The mass fraction of 8 times of amount is 25% barium chloride solution, is 30 DEG C in temperature, under conditions of revolving speed is 350r/min, is stirred
After 60min, filtering obtains filtrate, the metabisulfite solution in mass ratio 1 for being 35% by filtrate and parts by weight：2 mix, and are in temperature
30 DEG C, under conditions of revolving speed is 350r/min, after being stirred 60min, filtering, removal precipitating obtains modified glucose solution；It will
After mixed-powder calcines 15h, pretreatment powder batch is obtained, will pre-process powder batch and first use mass fraction is 15% salt pickling
It after washing 8 times, then is washed with deionized 10 times, and the pretreatment powder after washing is dried into 2h under the conditions of at a temperature of 90 °C
Afterwards, pretreatment powder is obtained, by pretreatment powder and water in mass ratio 1：15 are mixed in beaker, and pretreatment is added into beaker
The polyallylamine hydrochlorides that 0.6 times of powder quality obtain pretreatment powder under conditions of frequency is 55kHz after ultrasonic disperse 2h
Mixture, by pretreatment mixture of powders and silver nitrate in mass ratio 10：4 mixing, in temperature be 55 DEG C, revolving speed 400r/min
Under conditions of be stirred 40min after, filtering, obtain modified powder；By modified powder and modified glucose solution in mass ratio 1：
10 mixing are 65 DEG C in temperature, under conditions of revolving speed is 800r/min, after being stirred to react 2, then to modified powder and are modified grape
0.2 times of modified powder quality of sodium borohydride and the two of 0.2 times of modified powder quality hydration lemons are added in the mixture of sugar juice
Lemon acid sodium is 75 DEG C in temperature, and under conditions of revolving speed is 400r/min, after being stirred to react 3h, filtering must pre-process antibacterial addition
Agent；The sulfuric acid in mass ratio 1 for being 40% by titanium source solution and mass fraction：6 mixing, and to the mixture of titanium source solution and sulfuric acid
The middle pretreatment additive for being added 2 times of titanium source quality is 50 DEG C in temperature, under conditions of revolving speed is 400r/min, is stirred to react
After 8h, antibacterial additives mixture is obtained, after the pH to 7.5 that antibacterial additives mixture is adjusted with the ammonium hydroxide that mass fraction is 28%,
After being aged 15h under room temperature, filtering obtains filter cake, after filter cake is washed with deionized 10 times, and at a temperature of 90 °C
Under the conditions of dry 3h, obtain antibacterial additives；By polyethylene glycol and methylene chloride by volume 2：8 are mixed in blender, and to
0.3 times of polyethylene glycol volume of antibacterial additives and 1.4 times of polyethylene glycol volume of polylactic acid are added in blender, is in temperature
40 DEG C, under conditions of revolving speed is 400r/min, after being stirred 2h, and the ultrasonic disperse under conditions of frequency is 55kHz
30min obtains spinning solution, and spinning solution is formed a film through electrostatic spinning to get long acting antibiotic polylactic acid fiber membrane.The mixed-powder is
By titanium dioxide and potassium carbonate in molar ratio 4.0：1.5 mixed grindings, obtain mixed-powder.The calcination temperature is 850 DEG C.It is described
Titanium source solution is the potassium fluotitanate solution that mass fraction is 15%.The polyethylene glycol is polyethylene glycol 400.The electrostatic spinning
Condition is 22 ± 2kV of spinning voltage, receives distance 12cm, and fltting speed 1mL/h, air humidity 10%, temperature is room temperature,
Syringe needle internal diameter 0.6mm, uses aluminium foil as receiver used in spinning.The polylactic acid is the polylactic acid that molecular weight is 120000.
By polyallylamine hydrochlorides and modified glucose solution in mass ratio 1：10 mixing are 65 DEG C in temperature, and revolving speed is
Under conditions of 800r/min, after being stirred to react 2, then it is added into polyallylamine hydrochlorides and the mixture of modified glucose solution
The sodium borohydride and 0.2 times of polyallylamine hydrochlorides quality of trisodium citrate dihydrate that 0.2 times of polyallylamine hydrochlorides quality, in
Temperature is 75 DEG C, and under conditions of revolving speed is 400r/min, after being stirred to react 3h, filtering obtains pretreatment antibacterial additives；By titanium source
The sulfuric acid in mass ratio 1 that solution and mass fraction are 40%：6 mixing, and titanium source is added into the mixture of titanium source solution and sulfuric acid
The pretreatment additive that 2 times of quality is 50 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred to react 8h, obtains antibacterial
Additive agent mixture, after pH to 7.5 of the mass fraction for 28% ammonium hydroxide adjusting antibacterial additives mixture, in room temperature condition
After lower ageing 15h, filtering obtains filter cake, after filter cake is washed with deionized 10 times, and it is dry under the conditions of at a temperature of 90 °C
3h obtains antibacterial additives；By polyethylene glycol and methylene chloride by volume 2：8 are mixed in blender, and add into blender
Enter 0.3 times of polyethylene glycol volume of antibacterial additives and 1.4 times of polyethylene glycol volume of polylactic acid, in temperature be 40 DEG C, revolving speed
Under conditions of 400r/min, after being stirred 2h, and the ultrasonic disperse 30min under conditions of frequency is 55kHz, obtain spinning
Liquid forms a film spinning solution to get long acting antibiotic polylactic acid fiber membrane through electrostatic spinning.The calcination temperature is 850 DEG C.The titanium
Source solution is the potassium fluotitanate solution that mass fraction is 15%.The polyethylene glycol is polyethylene glycol 400.The Static Spinning strand
Part is 22 ± 2kV of spinning voltage, receives distance 12cm, and fltting speed 1mL/h, air humidity 10%, temperature is room temperature, is spun
Syringe needle internal diameter 0.6mm used in silk, uses aluminium foil as receiver.The polylactic acid is the polylactic acid that molecular weight is 120000.
After mixed-powder is calcined 15h, pretreatment powder batch is obtained, is first with mass fraction by pretreatment powder batch
It after salt acid elution 8 times of 15%, then is washed with deionized 10 times, and by the pretreatment powder after washing at a temperature of 90 °C
Under the conditions of after dry 2h, obtain pretreatment powder, will pretreatment powder and water in mass ratio 1：15 are mixed in beaker, and to beaker
The middle polyallylamine hydrochlorides that 0.6 times of powder quality of pretreatment is added, under conditions of frequency is 55kHz after ultrasonic disperse 2h,
Mixture of powders must be pre-processed, by pretreatment mixture of powders and silver nitrate in mass ratio 10：4 mixing are 55 DEG C in temperature, turn
After speed is stirred 40min under conditions of being 400r/min, filtering obtains modified powder；By modified powder in temperature be 65 DEG C, turn
Under conditions of speed is 800r/min, after being stirred to react 2, then 0.2 times of modified powder quality of hydroboration is added into modified powder
Sodium and 0.2 times of modified powder quality of trisodium citrate dihydrate are 75 DEG C in temperature, under conditions of revolving speed is 400r/min, stir
After mixing reaction 3h, filtering obtains pretreatment antibacterial additives；The sulfuric acid in mass ratio 1 for being 40% by titanium source solution and mass fraction：6
Mixing, and into the mixture of titanium source solution and sulfuric acid be added 2 times of titanium source quality pretreatment additive, in temperature be 50 DEG C,
Under conditions of revolving speed is 400r/min, after being stirred to react 8h, antibacterial additives mixture is obtained, the ammonium hydroxide for being 28% with mass fraction
After the pH to 7.5 for adjusting antibacterial additives mixture, after being aged 15h under room temperature, filtering obtains filter cake, filter cake is spent
After ion water washing 10 times, and the dry 3h under the conditions of at a temperature of 90 °C, obtain antibacterial additives；By polyethylene glycol and dichloromethane
Alkane by volume 2：8 are mixed in blender, and 0.3 times of polyethylene glycol volume of antibacterial additives are added into blender and gather
The polylactic acid that 1.4 times of ethylene glycol volume, in temperature be 40 DEG C, revolving speed be 400r/min under conditions of, after being stirred 2h, and in
Frequency is ultrasonic disperse 30min under conditions of 55kHz, obtains spinning solution, and spinning solution is formed a film through electrostatic spinning to get long acting antibiotic
Polylactic acid fiber membrane.The mixed-powder is by titanium dioxide and potassium carbonate in molar ratio 4.0：1.5 mixed grindings, obtain mixed powder
End.The calcination temperature is 850 DEG C.The titanium source solution is the potassium fluotitanate solution that mass fraction is 15%.The polyethylene glycol
For polyethylene glycol 400.The electrospinning conditions are 22 ± 2kV of spinning voltage, receive distance 12cm, fltting speed 1mL/h,
Air humidity is 10%, and temperature is room temperature, and syringe needle internal diameter 0.6mm, uses aluminium foil as receiver used in spinning.The polylactic acid is
The polylactic acid that molecular weight is 120000.
By glucose and Potassiumiodate in mass ratio 1：2 are mixed in flask, and 30 times of glucose quality are added into flask
Water, in temperature be 70 DEG C, revolving speed be 380r/min under conditions of, after being stirred to react 4h, then into flask be added grape saccharic
The mass fraction of 8 times of amount is 25% barium chloride solution, is 30 DEG C in temperature, under conditions of revolving speed is 350r/min, is stirred
After 60min, filtering obtains filtrate, the metabisulfite solution in mass ratio 1 for being 35% by filtrate and parts by weight：2 mix, and are in temperature
30 DEG C, under conditions of revolving speed is 350r/min, after being stirred 60min, filtering, removal precipitating obtains modified glucose solution；It will
After mixed-powder calcines 15h, pretreatment powder batch is obtained, will pre-process powder batch and first use mass fraction is 15% salt pickling
It after washing 8 times, then is washed with deionized 10 times, and the pretreatment powder after washing is dried into 2h under the conditions of at a temperature of 90 °C
Afterwards, pretreatment powder is obtained, by pretreatment powder and water in mass ratio 1：15 are mixed in beaker, and pretreatment is added into beaker
The polyallylamine hydrochlorides that 0.6 times of powder quality obtain pretreatment powder under conditions of frequency is 55kHz after ultrasonic disperse 2h
Mixture, by pretreatment mixture of powders and silver nitrate in mass ratio 10：4 mixing, in temperature be 55 DEG C, revolving speed 400r/min
Under conditions of be stirred 40min after, filtering, obtain modified powder；By polyethylene glycol and methylene chloride by volume 2：8 are mixed in
In blender, and 1.4 times of polyethylene glycol volume of polylactic acid is added into blender, in temperature be 40 DEG C, revolving speed 400r/
Under conditions of min, after being stirred 2h, and the ultrasonic disperse 30min under conditions of frequency is 55kHz, spinning solution is obtained, by spinning
Liquid forms a film through electrostatic spinning to get long acting antibiotic polylactic acid fiber membrane.The mixed-powder is to press titanium dioxide and potassium carbonate
Molar ratio 4.0：1.5 mixed grindings, obtain mixed-powder.The calcination temperature is 850 DEG C.The polyethylene glycol is polyethylene glycol
400.The electrospinning conditions are 22 ± 2kV of spinning voltage, receive distance 12cm, fltting speed 1mL/h, and air humidity is
10%, temperature is room temperature, and syringe needle internal diameter 0.6mm, uses aluminium foil as receiver used in spinning.The polylactic acid is that molecular weight is
120000 polylactic acid.
Comparative example：The long acting antibiotic polylactic acid fiber membrane of Wuxi material production Co., Ltd production.
Example 1 to the resulting long acting antibiotic polylactic acid fiber membrane of example 4 and comparative example product are subjected to performance detection, specifically
Detection method is as follows：
Antibiotic property：Improvement oscillation flask method is selected to be tested, strain, which is selected on nature and human skin and mucous membrane, to be distributed most
For extensive Staphylococcus aureus, Escherichia coli and Candida albicans.Test result bacteriostasis rate and bacteriostasis rate difference indicate,
The calculating of the two is respectively such as formula（1）It is shown：
Y=（Xa-Xb）/Xa·100% （1）
Specific testing result is as shown in table 1：
1 long acting antibiotic polylactic acid fiber membrane performance test results of table
By 1 testing result of table it is found that the long acting antibiotic polylactic acid fiber membrane of technical solution of the present invention preparation has excellent antibacterial
It the characteristics of performance and long acting antibiotic performance, has broad prospects in the development of environment-friendly materials technology industry.
Claims (8)
1. a kind of preparation method of long acting antibiotic polylactic acid fiber membrane, it is characterised in that：Specifically preparation step is：
（1）Mixed-powder is calcined, is washed, it is dry, pretreatment powder is obtained, by pretreatment powder and water in mass ratio 1：10~1：
15 mixing, and the polyallylamine hydrochlorides of 0.3~0.6 times of powder quality of pretreatment are added, after ultrasonic disperse, obtain pretreatment powder
Mixture, by pretreatment mixture of powders and silver nitrate in mass ratio 10：3~10：4 mixing, after being stirred, filtering must change
Property powder；
（2）By modified powder and modified glucose solution in mass ratio 1：6~1：10 mixing, after being stirred to react, add modification
The sodium borohydride and 0.1~0.2 times of modified powder quality of trisodium citrate dihydrate that 0.1~0.2 times of powder quality, are stirred to react
Afterwards, it filters, obtains pretreatment antibacterial additives；
（3）By titanium source solution and sulfuric acid in mass ratio 1：4~1：6 mixing, and 1~2 times of titanium source quality of pretreatment addition is added
Agent after being stirred to react, after adjusting pH to 7.0~7.5, is aged, filters, wash, dry, obtains antibacterial additives；
（4）By polyethylene glycol and methylene chloride by volume 2：7~2：8 mixing, and it is added 0.1~0.3 times of polyethylene glycol volume
Antibacterial additives and 1.0~1.4 times of polyethylene glycol volume of polylactic acid, after being stirred, ultrasonic disperse obtains spinning solution, will
Spinning solution forms a film through electrostatic spinning to get long acting antibiotic polylactic acid fiber membrane.
2. a kind of preparation method of long acting antibiotic polylactic acid fiber membrane according to claim 1, it is characterised in that：Step
（1）The mixed-powder is by titanium dioxide and potassium carbonate in molar ratio 4.0：1.3~4.0：1.5 mixed grindings, obtain mixed powder
End.
3. a kind of preparation method of long acting antibiotic polylactic acid fiber membrane according to claim 1, it is characterised in that：Step
（1）The calcination temperature is 750~850 DEG C.
4. a kind of preparation method of long acting antibiotic polylactic acid fiber membrane according to claim 1, it is characterised in that：Step
（2）The modified glucose mixed liquor is by glucose and Potassiumiodate in mass ratio 1：2 mixing, and be added glucose quality 20~
30 times of water after being stirred to react, is added 5~8 times of glucose quality of barium chloride solution, is stirred, filters, obtain filtrate, will
Filtrate and metabisulfite solution in mass ratio 1：2 mixing, filtering, removal precipitating obtain modified glucose mixed liquor.
5. a kind of preparation method of long acting antibiotic polylactic acid fiber membrane according to claim 1, it is characterised in that：Step
（3）The titanium tetrachloride that the titanium source solution is the potassium fluotitanate solution that mass fraction is 10~15% or mass fraction is 8~15%
Solution.
6. a kind of preparation method of long acting antibiotic polylactic acid fiber membrane according to claim 1, it is characterised in that：Step
（4）The polyethylene glycol is polyethylene glycol 400.
7. a kind of preparation method of long acting antibiotic polylactic acid fiber membrane according to claim 1, it is characterised in that：Step
（4）The electrospinning conditions are 22 ± 2kV of spinning voltage, receive distance 12cm, fltting speed 1mL/h, and air humidity is
10%, temperature is room temperature, and syringe needle internal diameter 0.6mm, uses aluminium foil as receiver used in spinning.
8. a kind of preparation method of long acting antibiotic polylactic acid fiber membrane according to claim 1, it is characterised in that：Step
（4）The polylactic acid is the polylactic acid that molecular weight is 100000~120000.
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| CN110328920A (en) * | 2019-06-21 | 2019-10-15 | 陈秀梅 | A kind of environment-friendly composite material and preparation method thereof for anti-toxic gas |
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