CN109610165A - A kind of preparation method of antibacterial photocatalysis flaxen fiber - Google Patents

A kind of preparation method of antibacterial photocatalysis flaxen fiber Download PDF

Info

Publication number
CN109610165A
CN109610165A CN201811191669.8A CN201811191669A CN109610165A CN 109610165 A CN109610165 A CN 109610165A CN 201811191669 A CN201811191669 A CN 201811191669A CN 109610165 A CN109610165 A CN 109610165A
Authority
CN
China
Prior art keywords
flaxen fiber
photocatalysis
antibacterial
preparation
fiber
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201811191669.8A
Other languages
Chinese (zh)
Other versions
CN109610165B (en
Inventor
杨龙
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hangzhou Chong Yi Electromechanical Technology Co Ltd
Original Assignee
Hangzhou Chong Yi Electromechanical Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hangzhou Chong Yi Electromechanical Technology Co Ltd filed Critical Hangzhou Chong Yi Electromechanical Technology Co Ltd
Priority to CN201811191669.8A priority Critical patent/CN109610165B/en
Publication of CN109610165A publication Critical patent/CN109610165A/en
Application granted granted Critical
Publication of CN109610165B publication Critical patent/CN109610165B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224Esters of carboxylic acids; Esters of carbonic acid
    • D06M13/2246Esters of unsaturated carboxylic acids
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Catalysts (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The present invention relates to flaxen fiber technical fields, solve the problem that fiber photocatalysis performance is bad, and photochemical catalyst causes oxidative degradation to cause fiber service life short fiber, disclose a kind of preparation method of antibacterial photocatalysis flaxen fiber.Flaxen fiber is first carried out steam shredding processing by this method, it is then immersed in olive polyphenol class extract solution, it is immersed in dopamine solution after taking-up and crosslinks reaction in one layer of three-dimensional cross-linked reticular structure of flaxen fiber surface formation, it is then immersed in pyromellitic trimethylsilyl chloride solution, pyromellitic trimethylsilyl chloride hydrolysis introduces carboxyl, is connected using the coordination of carboxyl and photochemical catalyst on flaxen fiber surface.Flaxen fiber prepared by the present invention has stronger photocatalysis performance, and photochemical catalyst will not cause Oxidative demage to fiber, and service life is longer.

Description

A kind of preparation method of antibacterial photocatalysis flaxen fiber
Technical field
The present invention relates to flaxen fiber technical fields, more particularly, to a kind of preparation method of antibacterial photocatalysis flaxen fiber.
Background technique
Photocatalysis is a kind of method of the degradation of contaminant of relative energy-saving, by utilizing sunlight can be complete effective Degradation of contaminant, catalysis material are energy needed for being converted to chemical reaction using luminous energy existing for nature under the irradiation of light Amount is the oxygen of surrounding and hydrone is excited into the free anion of great oxidability to generate catalytic action, itself does not rise The substance that variation can but promote chemical reaction to carry out, catalysis material have antibiotic property, air cleaning, deodorization, mould proof, anti- Algae, antifouling automatic cleaning action can almost decompose all organic substance base portions being harmful to the human body and divide inorganic substances.It is urged with the time Changing material has high safety, it might even be possible to which as food and medicine additive, while catalysis material provides only reaction Place, itself are simultaneously not involved in chemical reaction, have good persistence.In the prior art by the substance with photocatalysis It is public come catalyzing and degrading pollutant matter, such as China Patent Publication No. CN106012071 using fiber as carrier in conjunction with fiber A kind of continuous cellulose/TiO with photocatalysis performance is opened2Cellulose, is first configured to by the preparation method of airsetting glue fiber Titanium dioxide optical catalyst is added in spinning solution, and acid solution, ethanol solution or acetone soln are then added in coagulating basin and makees For coagulating bath, the spinning solution that titanium dioxide optical catalyst is added is added in coagulating bath, wet spinning is carried out, is contained The cellulose gel glue fiber of titanium dioxide optical catalyst, by fiber roll around room temperature ageing, uses deionized water in immersion aged solution Then washing carries out solvent displacement to neutrality, it is dry to get.To directly have photocatalysis in the technical solution of this patent disclosure The titanium dioxide of performance is mixed into spinning solution, then passes through spinning, coagulation forming, due to most of titanium dioxide in fiber after molding Titanium is located at the inside of fiber, and the titanium dioxide amount of fiber surface is less, and not only fiber photocatalysis performance is bad, also wastes more Titanium dioxide raw material, has extremely strong oxidation susceptibility additionally, due to titanium dioxide under light illumination, and titanium dioxide directly connects with fiber Touching will cause the oxidation of fiber, and the fracture of fibrous inside chemical bond is deteriorated so as to cause the mechanical property of fiber, shortens fiber Service life.
Summary of the invention
The present invention is to overcome prior art fiber photocatalysis performance bad, and light urges agent to cause oxidative degradation to lead fiber The problem for causing fiber service life short, provides a kind of preparation method of antibacterial photocatalysis flaxen fiber, flaxen fiber prepared by the present invention With stronger photocatalysis performance, photochemical catalyst will not cause Oxidative demage to fiber, and service life is longer.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of preparation method of antibacterial photocatalysis flaxen fiber, comprising the following steps:
1) by dopamine and ammonium persulfate 1:0.2-0.5 in mass ratio be added to pH value be 8.2-8.5 Tris-HCl buffering it is molten Stirring and dissolving in liquid obtains dopamine solution, spare;
2) mass concentration is added in olive polyphenol class extract is that dissolution is configured to olive polyphenol class in 60-85% ethanol water Extract solution, it is spare;
3) flaxen fiber is placed in water and impregnates 2-5h, then carry out high temperature steam treatment 10-20min, distillation is stood after being disposed It is dipped in olive polyphenol extract solution, sonic oscillation 5-10min, is dipped in dopamine solution after taking out flaxen fiber In, 5-10h is reacted at 50-65 DEG C, obtains flaxen fiber a;
4) flaxen fiber a is immersed in the pyromellitic trimethylsilyl chloride solution that mass concentration is 0.4-0.8%, reacts 1-2min, obtains fiber crops Fiber b;
5) modified titanium dioxide photocatalyst and dispersing agent are added to the water, stir evenly to form dispersion liquid, then by flaxen fiber b It immerses in dispersion liquid and reacts 3-5h at 40-50 DEG C, make to be washed with deionized after taking-up, be dried to obtain antibacterial photocatalysis fiber crops fibre Dimension.
The present invention first carries out steam shredding processing to flaxen fiber, the surface texture of flaxen fiber is destroyed, to make olive polyphenol Class extract enters inside flaxen fiber under the action of ultrasonic wave and is attached to flaxen fiber surface, then is dipped in dopamine solution In, due to having more active group amino on dopamine, there is more active phenol on olive polyphenol class extract molecule Hydroxyl, dopamine occurs auto polymerization and hands over olive polyphenol class extract molecule under the action of oxidant ammonium sulfate Connection, thus in one layer of flaxen fiber surface aggregate three-dimensional cross-linked reticular structure macromolecular, this three-dimensional cross-linked reticular structure macromolecular tool There is stronger stability, there is stronger stability, there is preferable heat-resisting and antioxidation, in the effect of photochemical catalyst Under be less likely to occur to degrade, even if Partial digestion occurs, be also not easy to fall off from fiber surface, this is because the present invention is to numb fine Dimension carried out steam treatment before modified, so that flaxen fiber is in loose condition (of surface), enters olive polyphenol class extract inside flaxen fiber, After polymerization crosslinking occurs for olive polyphenol class extract and dopamine, inside a part of polymer insertion flaxen fiber, to increase by three The bond strength for tieing up cross-linked structure macromolecular and flaxen fiber, makes it be not easy to fall off from flaxen fiber surface;On the other hand, olive Olive Polyphenols extract activity with higher has stronger bactericidal effect, inhibits growth and breeding of the bacterium on fiber, from And prevent decomposition destruction of the bacterium to fiber and polymer.
Olive polyphenol class extract is reacted in the three-dimensional cross-linked reticular structure molecule generated with dopamine with more The stronger amino of activity and hydroxyl group, amino and hydroxyl group can occur affine with the acid chloride groups on pyromellitic trimethylsilyl chloride Pyromellitic trimethylsilyl chloride is grafted on three-dimensional cross-linked reticular structure molecule by substitution reaction, is had neither part nor lot in pyromellitic trimethylsilyl chloride anti- Hydrolysis occurs in water and generates carboxyl for the acid chloride groups answered, can be with the Ti in photochemical catalyst titanium dioxide4+It is coordinated Effect assigns flaxen fiber photocatalysis performance so that photochemical catalyst is connected to flaxen fiber surface.Compared to the prior art (background Technical agency continues), since photochemical catalyst is connected to flaxen fiber surface, fibrous inside and insertion fibre are mixed into compared to by photochemical catalyst Dimension table face, greatly increases the contact area of photochemical catalyst and air, to increase photocatalysis efficiency and save the use of photochemical catalyst Amount.In addition olive polyphenol class extract reacts the three-dimensional cross-linked reticular structure macromolecular generated with dopamine and has compared with strong stability Property, it can prevent photochemical catalyst from contacting with flaxen fiber as layer protecting film on flaxen fiber surface, to prevent the oxygen of flaxen fiber Change degradation, extends the service life of flaxen fiber.
Preferably, dopamine solution solubility is 2-5wt% in the step 1).
Preferably, olive polyphenol class extract solution concentration is 5-15wt% in the step 2).
Preferably, sonic oscillation power is 100-200W in the step 3).
Preferably, solvent is n-hexane, toluene, one in hexamethylene in pyromellitic trimethylsilyl chloride solution in the step 4) Kind.
Preferably, modified titanium dioxide photocatalyst additive amount is the 5-10wt% of water, dispersing agent in the step 5) Additive amount is the 0.5-1wt% of water.
Preferably, dispersing agent is sodium tripolyphosphate, in calgon, sodium pyrophosphate, waterglass in the step 5) At least one.
Preferably, in the step 5) modified titanium dioxide photocatalyst preparation method the following steps are included:
Rodlike nano SiO 2 particle is added to the water to be uniformly mixed to form suspension, sulfuric acid is added into suspension The mass ratio of titanium, titanium sulfate and rodlike nano SiO 2 particle is 1:0.3-0.6,2-5h is stirred to react at 80-85 DEG C, so After be added epoxy silane coupling, stir 10-20min, stand 30-50min, be placed at 85-95 DEG C and evaporate, be dried to obtain and change Property titanium dioxide optical catalyst.
It is heated in water using titanium sulfate and generates nano-titanium dioxide precipitating, so that nanometer shape titanium dioxide be made to be incorporated in stick Shape nano-silica surface, two grade carriers of the rod-like nano silica as photochemical catalyst titanium dioxide, is received due to rodlike Rice silica is inorganic material, and the oxidisability of photochemical catalyst cannot damage it, is then coupled using epoxy radicals silicone hydride Rod-like nano silica is connected in the three-dimensional cross-linked reticular structure macromolecular on flaxen fiber surface (epoxy radicals silicone hydride coupling by agent The alkoxy of agent is connect with rod-like nano silica, on the epoxy ring-opening of the other end and three-dimensional cross-linked reticular structure macromolecular The carboxyl that pyromellitic trimethylsilyl chloride hydrolysis generates reacts, so that photochemical catalyst is connected on flaxen fiber), photochemical catalyst at this time There are the effects of two kinds of binding forces with flaxen fiber: first is that above-mentioned epoxy silane coupling is directly bonded to act on;Second is that dioxy Change the Ti in titanium4+It is formed with the carboxyl of pyromellitic trimethylsilyl chloride hydrolysis generation in flaxen fiber surface three dimension cross-linked structure macromolecular Coordination;To greatly improve the binding force of photochemical catalyst and flaxen fiber, photochemical catalyst is made to be not easy to fall off from fiber. Since titanium dioxide is attached on rod-like nano silica, to reduce titanium dioxide granule and three-dimensional cross-linked reticular structure is big Molecule contacts weaken photochemical catalyst to the oxidation of three-dimensional cross-linked reticular structure, further increase whole stability;This In it should be noted that using other shapes nano silica, as granular nanometer silica urges the two of agent as light Grade carrier can not reach technical effect of the invention, because the titanium dioxide on granular nanometer silica supports is easy It is in contact with three-dimensional cross-linked reticular structure macromolecular, to cause certain shadow to the stability of three-dimensional cross-linked reticular structure It rings.
Preferably, the shape nano SiO 2 particle additive amount is the 15-20wt% of water.
Preferably, the mass ratio of the epoxy silane coupling and rodlike nano SiO 2 particle is 1:15-20.
Therefore, the invention has the following beneficial effects:
Specific embodiment
Below by specific embodiment, technical scheme is described further.
In the present invention, if not refering in particular to, used raw material and equipment etc. are commercially available or commonly used in the art, Method in embodiment is unless otherwise instructed the conventional method of this field.
Embodiment 1
The preparation method of modified titanium dioxide photocatalyst the following steps are included:
Rodlike nano SiO 2 particle is added to the water to be uniformly mixed to form suspension, rodlike nano SiO 2 particle Additive amount is the 18wt% of water, and titanium sulfate, the matter of titanium sulfate and rodlike nano SiO 2 particle are then added into suspension Amount is stirred to react 3h, then by epoxy silane coupling and rodlike nano SiO 2 particle than being 1:0.45 at 83 DEG C Mass ratio is that epoxy silane coupling is added in 1:18, stirs 15min, stands 40min, be placed at 90 DEG C and evaporate, be dried to obtain Modified titanium dioxide photocatalyst.
A kind of preparation method of antibacterial photocatalysis flaxen fiber, comprising the following steps:
1) dopamine and ammonium persulfate 1:0.4 in mass ratio are added in the Tris-HCl buffer solution that pH value is 8.3 and are stirred Dissolution obtains the dopamine solution that solubility is 3.5wt%, spare;
It 2) is that be configured to concentration be 10wt% for dissolution in 70% ethanol water by olive polyphenol class extract addition mass concentration Olive polyphenol class extract solution, it is spare;
3) flaxen fiber is placed in water and impregnates 3h, then carry out high temperature steam treatment 15min, distilled after being disposed immediately by it It immerses in olive polyphenol extract solution, with the power sonic oscillation 8min of 150W, is dipped in dopamine after taking out flaxen fiber In solution, 8h is reacted at 60 DEG C, obtains flaxen fiber a;
4) pyromellitic trimethylsilyl chloride is dissolved in the pyromellitic trimethylsilyl chloride solution for being configured to that concentration is 0.6wt% in n-hexane solvent, Flaxen fiber a is immersed in pyromellitic trimethylsilyl chloride solution, 1.5min is reacted, obtains flaxen fiber b;
5) modified titanium dioxide photocatalyst and pentasodium triphosphate of dispersing agent are added to the water, modified titanium dioxide photocatalyst adds Dosage is the 8wt% of water, and dispersing agent additive amount is the 0.7wt% of water, stirs evenly to form dispersion liquid, then soaks flaxen fiber b Enter and react 4h in dispersion liquid at 45 DEG C, makes to be washed with deionized after taking-up, is dried to obtain antibacterial photocatalysis flaxen fiber.
Embodiment 2
The preparation method of modified titanium dioxide photocatalyst the following steps are included:
Rodlike nano SiO 2 particle is added to the water to be uniformly mixed to form suspension, rodlike nano SiO 2 particle Additive amount is the 16wt% of water, and titanium sulfate, the matter of titanium sulfate and rodlike nano SiO 2 particle are then added into suspension Amount is stirred to react 2.5h, then by epoxy silane coupling and rodlike nano SiO 2 particle than being 1:0.35 at 81 DEG C Mass ratio be that epoxy silane coupling is added in 1:16, stir 12min, stand 35min, be placed at 86 DEG C evaporation, dry To modified titanium dioxide photocatalyst.
A kind of preparation method of antibacterial photocatalysis flaxen fiber, comprising the following steps:
1) dopamine and ammonium persulfate 1:0.25 in mass ratio are added in the Tris-HCl buffer solution that pH value is 8.2 and are stirred Dissolution obtains the dopamine solution that solubility is 2.5wt%, spare;
It 2) is that be configured to concentration be 6wt% olive for dissolution in 70% ethanol water by olive polyphenol class extract addition mass concentration Olive Polyphenols extract solution, it is spare;
3) flaxen fiber is placed in water and impregnates 2.5h, then carry out high temperature steam treatment 12min, distillation immediately will after being disposed It is immersed in olive polyphenol extract solution, with the power sonic oscillation 6min of 100W, is dipped in DOPA after taking out flaxen fiber In amine aqueous solution, 6h is reacted at 52 DEG C, obtains flaxen fiber a;
4) pyromellitic trimethylsilyl chloride is dissolved in the pyromellitic trimethylsilyl chloride solution for being configured to that concentration is 0.5wt% in toluene solvant, it will Flaxen fiber a immerses in pyromellitic trimethylsilyl chloride solution, reacts 1.5min, obtains flaxen fiber b;
5) modified titanium dioxide photocatalyst and sodium hexametaphosphate dispersant are added to the water, modified titanium dioxide photocatalyst adds Dosage is the 6wt% of water, and dispersing agent additive amount is the 0.6wt% of water, stirs evenly to form dispersion liquid, then soaks flaxen fiber b Enter and react 3.5h in dispersion liquid at 41 DEG C, makes to be washed with deionized after taking-up, is dried to obtain antibacterial photocatalysis flaxen fiber.
Embodiment 3
The preparation method of modified titanium dioxide photocatalyst the following steps are included:
Rodlike nano SiO 2 particle is added to the water to be uniformly mixed to form suspension, rodlike nano SiO 2 particle Additive amount is the 18wt% of water, and titanium sulfate, the matter of titanium sulfate and rodlike nano SiO 2 particle are then added into suspension Amount is stirred to react 4.5h, then by epoxy silane coupling and rodlike nano SiO 2 particle than being 1:0.5 at 84 DEG C Mass ratio be that epoxy silane coupling is added in 1:19, stir 18min, stand 45min, be placed at 92 DEG C evaporation, dry To modified titanium dioxide photocatalyst.
A kind of preparation method of antibacterial photocatalysis flaxen fiber, comprising the following steps:
1) dopamine and ammonium persulfate 1:0.45 in mass ratio are added in the Tris-HCl buffer solution that pH value is 8.4 and are stirred Dissolution obtains the dopamine solution that solubility is 4.5wt%, spare;
It 2) is that be configured to concentration be 12wt% for dissolution in 70% ethanol water by olive polyphenol class extract addition mass concentration Olive polyphenol class extract solution, it is spare;
3) flaxen fiber is placed in water and impregnates 4.5h, then carry out high temperature steam treatment 18min, distillation immediately will after being disposed It is immersed in olive polyphenol extract solution, with the power sonic oscillation 9min of 180W, is dipped in DOPA after taking out flaxen fiber In amine aqueous solution, 8h is reacted at 63 DEG C, obtains flaxen fiber a;
4) pyromellitic trimethylsilyl chloride is dissolved in the pyromellitic trimethylsilyl chloride solution for being configured to that concentration is 0.7wt% in cyclohexane solvent, Flaxen fiber a is immersed in pyromellitic trimethylsilyl chloride solution, 2min is reacted, obtains flaxen fiber b;
5) modified titanium dioxide photocatalyst and dispersing agent sodium pyrophosphate are added to the water, modified titanium dioxide photocatalyst addition Amount is the 9wt% of water, and dispersing agent additive amount is the 0.8wt% of water, stirs evenly to form dispersion liquid, then immerses flaxen fiber b 4.5h is reacted in dispersion liquid at 48 DEG C, makes to be washed with deionized after taking-up, be dried to obtain antibacterial photocatalysis flaxen fiber.
Embodiment 4
The preparation method of modified titanium dioxide photocatalyst the following steps are included:
Rodlike nano SiO 2 particle is added to the water to be uniformly mixed to form suspension, rodlike nano SiO 2 particle Additive amount is the 20wt% of water, and titanium sulfate, the matter of titanium sulfate and rodlike nano SiO 2 particle are then added into suspension Amount is stirred to react 5h, then by epoxy silane coupling and rodlike nano SiO 2 particle than being 1:0.6 at 85 DEG C Mass ratio is that epoxy silane coupling is added in 1:20, stirs 20min, stands 50min, be placed at 95 DEG C and evaporate, be dried to obtain Modified titanium dioxide photocatalyst.
A kind of preparation method of antibacterial photocatalysis flaxen fiber, comprising the following steps:
1) dopamine and ammonium persulfate 1:0.5 in mass ratio are added in the Tris-HCl buffer solution that pH value is 8.5 and are stirred Dissolution obtains the dopamine solution that solubility is 5wt%, spare;
It 2) is that be configured to concentration be 15wt% for dissolution in 85% ethanol water by olive polyphenol class extract addition mass concentration Olive polyphenol class extract solution, it is spare;
3) flaxen fiber is placed in water and impregnates 5h, then carry out high temperature steam treatment 20min, distilled after being disposed immediately by it It immerses in olive polyphenol extract solution, with the power sonic oscillation 10min of 200W, is dipped in dopamine after taking out flaxen fiber In solution, 10h is reacted at 65 DEG C, obtains flaxen fiber a;
4) pyromellitic trimethylsilyl chloride is dissolved in the pyromellitic trimethylsilyl chloride solution for being configured to that concentration is 0.8wt% in n-hexane solvent, Flaxen fiber a is immersed in pyromellitic trimethylsilyl chloride solution, 2min is reacted, obtains flaxen fiber b;
5) modified titanium dioxide photocatalyst and dispersing agent waterglass are added to the water, modified titanium dioxide photocatalyst additive amount For the 10wt% of water, dispersing agent additive amount is the 1wt% of water, stirs evenly to form dispersion liquid, then immerses flaxen fiber b and divides 5h is reacted in dispersion liquid at 50 DEG C, makes to be washed with deionized after taking-up, be dried to obtain antibacterial photocatalysis flaxen fiber.
Embodiment 5
The preparation method of modified titanium dioxide photocatalyst the following steps are included:
Rodlike nano SiO 2 particle is added to the water to be uniformly mixed to form suspension, rodlike nano SiO 2 particle Additive amount is the 15wt% of water, and titanium sulfate, the matter of titanium sulfate and rodlike nano SiO 2 particle are then added into suspension Amount is stirred to react 2h, then by epoxy silane coupling and rodlike nano SiO 2 particle than being 1:0.3 at 80 DEG C Mass ratio is that epoxy silane coupling is added in 1:15, stirs 10min, stands 30min, be placed at 85 DEG C and evaporate, be dried to obtain Modified titanium dioxide photocatalyst.
A kind of preparation method of antibacterial photocatalysis flaxen fiber, comprising the following steps:
1) dopamine and ammonium persulfate 1:0.2 in mass ratio are added in the Tris-HCl buffer solution that pH value is 8.2 and are stirred Dissolution obtains the dopamine solution that solubility is 2wt%, spare;
It 2) is that be configured to concentration be 5wt% olive for dissolution in 60% ethanol water by olive polyphenol class extract addition mass concentration Olive Polyphenols extract solution, it is spare;
3) flaxen fiber is placed in water and impregnates 2h, then carry out high temperature steam treatment 10min, distilled after being disposed immediately by it It immerses in olive polyphenol extract solution, with the power sonic oscillation 5min of 100W, is dipped in dopamine after taking out flaxen fiber In solution, 5h is reacted at 50 DEG C, obtains flaxen fiber a;
4) pyromellitic trimethylsilyl chloride is dissolved in the pyromellitic trimethylsilyl chloride solution for being configured to that concentration is 0.4wt% in toluene solvant, it will Flaxen fiber a immerses in pyromellitic trimethylsilyl chloride solution, reacts 1min, obtains flaxen fiber b;
5) modified titanium dioxide photocatalyst and pentasodium triphosphate of dispersing agent are added to the water, modified titanium dioxide photocatalyst adds Dosage is the 5wt% of water, and dispersing agent additive amount is the 0.5wt% of water, stirs evenly to form dispersion liquid, then soaks flaxen fiber b Enter and react 3h in dispersion liquid at 40 DEG C, makes to be washed with deionized after taking-up, is dried to obtain antibacterial photocatalysis flaxen fiber.
Experimental test:
1h is radiated to the rhdamine B and methylene blue dye that dye strength is 6ppm respectively using ultraviolet radiation, then Detect pollutant degradation efficiency, used in ultraviolet wavelength be 365nm, radiosity 7.6mw/cm2, fiber The dosage of photochemical catalyst is 1g/L.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification It is right according to the technical essence of the invention for the equivalent embodiment of equivalent variations, but without departing from the technical solutions of the present invention Any simple modification, equivalent change and modification made by above embodiments, all of which are still within the scope of the technical scheme of the invention.

Claims (10)

1. a kind of preparation method of antibacterial photocatalysis flaxen fiber, which comprises the following steps:
1) by dopamine and ammonium persulfate 1:0.2-0.5 in mass ratio be added to pH value be 8.2-8.5 Tris-HCl buffering it is molten Stirring and dissolving in liquid obtains dopamine solution, spare;
2) mass concentration is added in olive polyphenol class extract is that dissolution is configured to olive polyphenol class in 60-85% ethanol water Extract solution, it is spare;
3) flaxen fiber is placed in water and impregnates 2-5h, then carry out high temperature steam treatment 10-20min, distillation is stood after being disposed It is dipped in olive polyphenol extract solution, sonic oscillation 5-10min, is dipped in dopamine solution after taking out flaxen fiber In, 5-10h is reacted at 50-65 DEG C, obtains flaxen fiber a;
4) flaxen fiber a is immersed in the pyromellitic trimethylsilyl chloride solution that mass concentration is 0.4-0.8%, reacts 1-2min, obtain numb fibre Tie up b;
5) modified titanium dioxide photocatalyst and dispersing agent are added to the water, stir evenly to form dispersion liquid, then by flaxen fiber b It immerses in dispersion liquid and reacts 3-5h at 40-50 DEG C, make to be washed with deionized after taking-up, be dried to obtain antibacterial photocatalysis fiber crops fibre Dimension.
2. a kind of preparation method of antibacterial photocatalysis flaxen fiber according to claim 1, which is characterized in that the step 1) Middle dopamine solution solubility is 2-5wt%.
3. a kind of preparation method of antibacterial photocatalysis flaxen fiber according to claim 1, which is characterized in that the step 2 Middle olive polyphenol class extract solution concentration is 5-15wt%.
4. a kind of preparation method of antibacterial photocatalysis flaxen fiber according to claim 1, which is characterized in that the step 3) Middle sonic oscillation power is 100-200W.
5. a kind of preparation method of antibacterial photocatalysis flaxen fiber according to claim 1, which is characterized in that the step 4) Solvent is one of n-hexane, toluene, hexamethylene in middle pyromellitic trimethylsilyl chloride solution.
6. a kind of preparation method of antibacterial photocatalysis flaxen fiber according to claim 1, which is characterized in that the step 5) Middle modified titanium dioxide photocatalyst additive amount is the 5-10wt% of water, and dispersing agent additive amount is the 0.5-1wt% of water.
7. a kind of preparation method of antibacterial photocatalysis flaxen fiber according to claim 1, which is characterized in that the step 5) Middle dispersing agent is at least one of sodium tripolyphosphate, calgon, sodium pyrophosphate, waterglass.
8. a kind of preparation method of antibacterial photocatalysis flaxen fiber according to claim 1, which is characterized in that the step 5) The preparation method of middle modified titanium dioxide photocatalyst the following steps are included:
Rodlike nano SiO 2 particle is added to the water to be uniformly mixed to form suspension, sulfuric acid is added into suspension The mass ratio of titanium, titanium sulfate and rodlike nano SiO 2 particle is 1:0.3-0.6,2-5h is stirred to react at 80-85 DEG C, so After be added epoxy silane coupling, stir 10-20min, stand 30-50min, evaporated at 85-95 DEG C, be dried to obtain modification Titanium dioxide optical catalyst.
9. a kind of preparation method of antibacterial photocatalysis flaxen fiber according to claim 8, which is characterized in that described rodlike two Silica nano particle additive amount is the 15-20wt% of water.
10. a kind of preparation method of antibacterial photocatalysis flaxen fiber according to claim 8, which is characterized in that the epoxy The mass ratio of base silane coupling agent and rodlike nano SiO 2 particle is 1:15-20.
CN201811191669.8A 2018-10-12 2018-10-12 Preparation method of antibacterial photocatalytic fibrilia Active CN109610165B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811191669.8A CN109610165B (en) 2018-10-12 2018-10-12 Preparation method of antibacterial photocatalytic fibrilia

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811191669.8A CN109610165B (en) 2018-10-12 2018-10-12 Preparation method of antibacterial photocatalytic fibrilia

Publications (2)

Publication Number Publication Date
CN109610165A true CN109610165A (en) 2019-04-12
CN109610165B CN109610165B (en) 2021-04-20

Family

ID=66002371

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811191669.8A Active CN109610165B (en) 2018-10-12 2018-10-12 Preparation method of antibacterial photocatalytic fibrilia

Country Status (1)

Country Link
CN (1) CN109610165B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111979765A (en) * 2019-05-23 2020-11-24 苏州合祥纺织科技有限公司 Preparation method of hydroxyl fiber with antibacterial function
CN112726206A (en) * 2020-12-28 2021-04-30 安徽省临泉县万隆塑料包装有限公司 Ultraviolet-resistant polyethylene non-woven fabric and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101725034A (en) * 2009-12-10 2010-06-09 东华大学 Method for preparing Au modified and TiO2 compound air purified functional textile at low temperature in situ
US20100166870A1 (en) * 2006-12-21 2010-07-01 The University Of Western Australia Method for Coating Nanoparticles
CN102153779A (en) * 2011-03-04 2011-08-17 浙江理工大学 Anti-aging method for polymer materials
CN106215717A (en) * 2016-08-05 2016-12-14 浙江理工大学 A kind of preparation method of compound PVDF ultrafiltration membrane
CN108380063A (en) * 2018-02-27 2018-08-10 天津大学 A kind of preparation method of nano titanium dioxide hybrid composite nanometer filtering film
CN109012188A (en) * 2018-09-09 2018-12-18 郑州成济堂生物科技有限公司 A kind of preparation method of high-flux composite nanofiltration membrane

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100166870A1 (en) * 2006-12-21 2010-07-01 The University Of Western Australia Method for Coating Nanoparticles
CN101725034A (en) * 2009-12-10 2010-06-09 东华大学 Method for preparing Au modified and TiO2 compound air purified functional textile at low temperature in situ
CN102153779A (en) * 2011-03-04 2011-08-17 浙江理工大学 Anti-aging method for polymer materials
CN106215717A (en) * 2016-08-05 2016-12-14 浙江理工大学 A kind of preparation method of compound PVDF ultrafiltration membrane
CN108380063A (en) * 2018-02-27 2018-08-10 天津大学 A kind of preparation method of nano titanium dioxide hybrid composite nanometer filtering film
CN109012188A (en) * 2018-09-09 2018-12-18 郑州成济堂生物科技有限公司 A kind of preparation method of high-flux composite nanofiltration membrane

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
何建新主编: "《新型纤维材料学》", 31 July 2014, 东华大学出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111979765A (en) * 2019-05-23 2020-11-24 苏州合祥纺织科技有限公司 Preparation method of hydroxyl fiber with antibacterial function
CN111979765B (en) * 2019-05-23 2022-10-25 苏州合祥纺织科技有限公司 Preparation method of hydroxyl fiber with antibacterial function
CN112726206A (en) * 2020-12-28 2021-04-30 安徽省临泉县万隆塑料包装有限公司 Ultraviolet-resistant polyethylene non-woven fabric and preparation method thereof

Also Published As

Publication number Publication date
CN109610165B (en) 2021-04-20

Similar Documents

Publication Publication Date Title
CN109610165A (en) A kind of preparation method of antibacterial photocatalysis flaxen fiber
CN105295105B (en) A kind of bacteria cellulose based composites with photocatalysis antibacterial
CN103464217A (en) Alginate-based composite hydrogel catalytic membrane of renewable catalyst and preparation method thereof
CN105344328B (en) A kind of preparation method of cotton fiber carried titanium dioxide composite material film
CN105413753A (en) Preparation method of bast fiber-carried titanium dioxide composite material powder
CN106567192A (en) Method for preparing multifunctional health-care nanofiber membrane
CN102174505B (en) Preparation method of granular carrier immobilized bienzyme for treating papermaking white water
CN104975366A (en) Lyocell fiber containing nano particles and preparation method thereof
CN106589411B (en) A kind of pineapple bran carboxymethyl cellulose/polyvinyl alcohol/mesoporous silicon oxide composite hydrogel and the preparation method and application thereof
CN105540724B (en) A kind of NEW TYPE OF COMPOSITE decolorising agent and its waste water decoloring processing method using NEW TYPE OF COMPOSITE decolorising agent
CN103332737A (en) Preparation method of titanium dioxide nano-powder
CN112267291A (en) Production process of nano zinc oxide antibacterial fabric
CN107312204B (en) For removing chitosan ferrotitanium polymeric material and its preparation of organic matter of sewage
CN113003644B (en) Environment-friendly deodorant and preparation method thereof
CN102061618A (en) Method for grafting mesoporous silica gel on fiber through calcium ion crosslinking
CN112680036A (en) Photocatalytic formaldehyde-removing coating and preparation method thereof
CN110871099A (en) Ag-containing material3PO4And carboxylated g-C3N4Preparation method of photocatalytic degradation nano-fiber
CN114058055B (en) Production method of degradable frozen food packaging film with photo-thermal antibacterial function
CN109319899A (en) A kind of preparation method of environment friendly biological base flocculant
CN112044405B (en) Medical wastewater treating agent and preparation method thereof
CN109354935A (en) A kind of mould proof diatom ooze coating of resistant and preparation method thereof
CN1559672A (en) Preparation method of titanium dioxide photo catalyst composite solution
CN103587182B (en) Preparation method of PVA/NCC-TiO2/PVA composite membrane
CN106362686A (en) Preparation method of composite material for gathering and degrading benzene series organic wastewater
CN108456135B (en) Method for recycling colored waste polyester-cotton fibers

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant