CN109778336A - The polyacrylonitrile fibre and its preparation method of a kind of sustained-release antibacterial and application - Google Patents
The polyacrylonitrile fibre and its preparation method of a kind of sustained-release antibacterial and application Download PDFInfo
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- CN109778336A CN109778336A CN201811594085.5A CN201811594085A CN109778336A CN 109778336 A CN109778336 A CN 109778336A CN 201811594085 A CN201811594085 A CN 201811594085A CN 109778336 A CN109778336 A CN 109778336A
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Abstract
The invention discloses polyacrylonitrile fibres of a kind of sustained-release antibacterial and the preparation method and application thereof.The preparation method is that: using plant cellulose as raw material, is handled for several times through ultra micron pulverizer, prepare nano-cellulose；Then with the C2 in periodate oxidized cellulose glucopyranose structural unit, the position C3 produces aldehyde radical；The nano-cellulose of nano-Ag particles load is generated after aldocellulose and silver ammino solution are reacted under heating environment；The nano-cellulose that nano-Ag particles load is doped in polyacrylonitrile spinning solution, the polyacrylonitrile fibre of sustained-release antibacterial is obtained after wet spinning, drawing-off, washing and drying process.The polyacrylonitrile fibre of the sustained-release antibacterial not only has good antibacterial effect, and tensile strength is greatly improved, dyeability and hygroscopicity have improvement, may be used on the functional spinning material such as anti-biotic material, flat polyacrylonitrile fibre, high modulus polypropylene nitrile fiber, rub resistance acrylic fiber and textile field.
Description
Technical field
The invention belongs to antibacterial fabric fields, and in particular to a kind of polyacrylonitrile fibre of sustained-release antibacterial and its preparation side
Method and application.
Background technique
Acrylic fiber has the title of artificial wool, has soft, bulk, easy dye, bright in colour, fast light, antibacterial, is not afraid of and damages by worms
The advantages that.Acrylic fiber mainly make it is civilian, can it is pure spin it is also blended, a variety of woollens, knitting wool, woollen blanket, gym suit is made, can also people
Fur, plush, buiky yarn, rotary hose, sunshade cloth etc. are made, textile is widely used in the neck such as clothes, decoration, industry
Domain.Acrylic fibers are very unique in internal macromolecular ordered arrangement structure, are in irregular helical conformation, and not stringent crystallization
Area.Pure polyacrylonitrile fibre hygroscopicity is poor, and dyeing is difficult.Traditional anti-bacterial fibre mostly uses dipping absorption method, though technique
Simply, but washability is poor, and antibacterial agent waste greatly, pollutes environment.Therefore, a kind of polyacrylonitrile fibre of sustained-release antibacterial is developed
It is worth with highly important economy and society.
Nano-cellulose is a kind of natural organic high-molecular material with higher order structures that diameter is less than 100nm.
Surface oxygen-containing functional group rich in is easily chemically modified or modifies preparation cellulose derivative, to synthesize functionality
High molecular material.Published acrylic fibers related patents report has focused largely on the functionalization aspect of acrylic fiber at present, such as fire-retardant
Property (Chinese Patent Application No. 2015101883251), anti-pilling (Chinese Patent Application No. 2012103590942), antibiotic property
(Chinese Patent Application No. 2016104843744), ultraviolet-resistent property (Chinese Patent Application No. 2015104585036) and electric conductivity
(Chinese Patent Application No. 2008100742254) etc.；But it there is no load silver nanoparticle using about modified nanometer cellulose at present
The report of the acrylic fiber of the directly blended preparation sustained-release antibacterial of particle.
Summary of the invention
In order to overcome the disadvantages and deficiencies of the prior art, the primary purpose of the present invention is that providing a kind of gathering for sustained-release antibacterial
Dralon；
Another object of the present invention is to provide the preparation methods of the polyacrylonitrile fibre of above-mentioned sustained-release antibacterial；
Another object of the present invention is the application of the polyacrylonitrile fibre of above-mentioned sustained-release antibacterial.
The purpose of the invention is achieved by the following technical solution:
A kind of preparation method of the polyacrylonitrile fibre of sustained-release antibacterial, includes the following steps:
(1) it using plant fiber as raw material, is handled with ultra micron pulverizer and obtains nano-cellulose afterwards for several times；
(2) with the C2 in the nano-cellulose of periodate oxidation step (1) preparation in glucopyranose structural unit
With the position C3, the cellulose with 2,3- dialdehyde based structures is generated；
(3) by step (2) with 2,3- dialdehyde based structures cellulose and silver ammino solution reacted under heating environment
The nano-cellulose of nano-Ag particles load is generated after a period of time；
(4) nano-cellulose by the nano-Ag particles load in step (3) is added into poly- third according to certain mass ratio
Alkene nitrile spinning solution, wet spinning, the polyacrylonitrile that sustained-release antibacterial is obtained after drawing-off, washing and drying are fine after mixing
Dimension.
Preferably, plant fiber described in step (1) can be the lumber fibres such as aspen fibers by using silicon, Eucalyptus Fibers, pine cellulosic,
And at least one in the non-wood fibrous raw materials such as rice-straw fibre, straw fiber, reed fiber, cornstalk fibers, bamboo fiber
Kind.
Preferably, ultra micron pulverizer treatment conditions described in step (1) are as follows: disk mill gap is -100~200 μm, processing
Number is 10~100 times.
Preferably, periodate oxidation condition described in step (2) are as follows: periodate 1 is added in every gram of nano-cellulose
~5g, is protected from light 1~3h at 40~80 DEG C, and mixing speed is 100~1000r/min.
Preferably, step (3) the silver ammino solution concentration is 0.01~0.5mol/L, the fibre with 2,3- dialdehyde based structures
The mass ratio of dimension element and silver ammino solution is 1:(10~500)；Silver-colored ammonia heats reaction condition are as follows: and temperature is 40~80 DEG C, reaction 5~
60min。
Preferably, polypropylene in the nano-cellulose and polyacrylonitrile spinning solution that nano-Ag particles load in step (4)
The mass ratio of nitrile is 1:(1~1000), 1~5h is stirred with the mixing speed of 100~1000r/min and is uniformly mixed；Drawing-off times
Rate is 1~30 times, drying temperature is 30~130 DEG C.
The polyacrylonitrile fibre of above-mentioned sustained-release antibacterial not only has good antibacterial effect, and tensile strength has very greatly
Raising, can be applied to anti-biotic material, flat polyacrylonitrile fibre, high modulus polypropylene nitrile fiber, rub resistance acrylic fiber
Deng the functional various fields such as spinning material and textile.
The preparation process of the polyacrylonitrile fibre of sustained-release antibacterial of the present invention is as shown in Figure 1.
The present invention has the following advantages and effects with respect to the prior art:
The invention firstly uses the positions C2, C3 in periodate selective oxidation cellulose molecular structure to obtain two aldehyde
Based structures construct 2,3- dicyano nano-cellulose；Redox reaction occurs in silver ammino solution using aldehyde radical, in nanometer
Cellulose surface equably generates nano-Ag particles.Then nano-Ag particles nano-cellulose and polyacrylonitrile spinning solution is straight
It connects to be uniformly mixed and carries out wet spinning, obtain the polyacrylonitrile fibre of sustained-release antibacterial.During the preparation process, in nano-cellulose
The hydroxyl of the position C2, C3 is aldehyde radical through periodate selective paraffin oxidation, and then is converted into carboxyl during silver mirror reaction, is provided
The indispensable active site for generating nano silver, improves the slow-release capability of silver ion.And due to the nano-catalytic of nano-cellulose
Effect can be convenient nano silver and efficiently, equably be assembled into nano-cellulose molecule.
The present invention not only expands the purposes of nano-cellulose, and is silver-carrying nano cellulose anti-biotic material in polyacrylonitrile
A kind of approach being simple and efficient is provided in terms of the preparation and application of fiber.The overall process of nano silver reduction is not added other and is urged
Agent, end-capping reagent and dispersing agent, this method are that have to delay by the preparation of environmentally protective synthetic method using natural organic fiber element
Release the polyacrylic fibre of anti-microbial property.
In addition, the introducing of the nano-cellulose of nano-silver loaded, since convert aldehyde groups are hydrophilic in oxidation-reduction process
Property carboxyl, facilitate improve virgin pp nitrile fiber hydroscopicity.Be added in polyacrylonitrile fibre containing abundant carboxyl and
The nano-cellulose of the nano-silver loaded of hydroxy functional group is easily colored since its chemical functional group's reactivity is higher, can be
Solve the problems, such as that the stock-dye of virgin pp nitrile is difficult to a certain extent.
Finally, the nano-cellulose of nano-silver loaded realizes orderly rearrangement in drafting process, and introduce a large amount of new
Hydrogenbond greatly improves the mechanical property of polyacrylonitrile fibre.
The preparation manipulation process of the nano-cellulose of nano-silver loaded of the present invention is simple, is easy to industrialization, has huge
Potential age deduction and social benefit.
Detailed description of the invention
Fig. 1 is the preparation process schematic diagram of the polyacrylonitrile fibre of sustained-release antibacterial.
Fig. 2 be 4 gained sustained-release antibacterial of virgin pp nitrile fiber and embodiment polyacrylonitrile fibre when breaking the plane of disruption
FE-SEM figure；Wherein a, b are respectively the sectional view and high magnification map of virgin pp nitrile fiber, and c, d are respectively 4 institute of embodiment
Obtain the sectional view and high magnification map of the polyacrylonitrile fibre of sustained-release antibacterial.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Polyacrylonitrile spinning solution described in embodiment is that polyacrylonitrile is dissolved in the sodium thiocyanate water solution of 60wt%
Obtained spinning solution, wherein the solid content of polyacrylonitrile is 13%.
In following embodiment, extension test and antibacterial test method are as follows:
Monfil extension test is carried out according to GB/T 31290-2014, and single fiber sample is cut into 10cm long, is used
LLY-06ED type electronic mono-fiber strong force instrument is tested, and is surveyed five times and is found out average value.
Anti-microbial property refers to GB/T 20944.3-2008, using concussion flask method test polyacrylonitrile fibre to large intestine bar
The antibacterial effect of bacterium (CMCC-44817) and staphylococcus aureus (CMCC-26003) counts fiber by colony counting method and exists
The bacterium of dipping concussion front and back reduces quantity and calculates antibiotic rate in bacterium mixed liquor, and calculation formula is as follows:
Antibiotic rate=(Q1-Q2)/Q1× 100%
Q1And Q2Respectively indicate the Escherichia coli quantity that anti-bacterial fibre is added into bacterial suspension concussion front and back.
Room temperature in embodiment when experimental implementation is 25 ± 1 DEG C.
Embodiment 1
A kind of polyacrylonitrile fibre of sustained-release antibacterial, preparation method are as follows:
(1) it using bamboo fiber as raw material, is handled with ultra micron pulverizer and obtains nano-cellulose afterwards for several times.Ultra micron mill
Treatment conditions are as follows: dense slurry is 0.1%, and disk mill gap is -100 μm, and number of processes is 10 times.
(2) C2 in the nano-cellulose for using sodium periodate oxidation step (1) to prepare in glucopyranose structural unit,
The position C3 generates the cellulose with 2,3- dialdehyde based structures.Sodium periodate oxidation condition are as follows: be added in every gram of nano-cellulose
Sodium metaperiodate 5g is protected from light 1h, mixing speed 500r/min at 80 DEG C.
(3) by step (2) aldocellulose and silver ammino solution react to generate after a period of time under heating environment and receive
The nano-cellulose of rice Argent grain load.Silver mirror reaction condition are as follows: silver ammino solution concentration be 0.01mol/L, aldocellulose with
The mass ratio of silver ammino solution is 1:500, and temperature is 40 DEG C, reacts 60min.
(4) nano-cellulose by the nano-Ag particles load in step (3) is added into poly- third according to certain mass ratio
Alkene nitrile spinning solution, wet spinning, the polyacrylonitrile that sustained-release antibacterial is obtained after drawing-off, washing and drying are fine after mixing
Dimension.The nano-cellulose of nano-Ag particles load and the mass ratio of polyacrylonitrile are 1:1000, with the stirring speed of 100r/min
Degree stirring 5h is uniformly mixed, and draft ratio is 1 times, drying temperature is 130 DEG C.
It is tested by omnipotent mechanical stretch machine and antibacterial tests, the tensile strength of the polyacrylonitrile fibre of the present embodiment is
2.6cN/dtex, the antibiotic rate to Escherichia coli and staphylococcus aureus are respectively 68% and 79%.
Embodiment 2
A kind of polyacrylonitrile fibre of sustained-release antibacterial, preparation method are as follows:
(1) it using Eucalyptus Fibers as raw material, is handled with ultra micron pulverizer and obtains nano-cellulose afterwards for several times.Ultra micron mill
Treatment conditions are as follows: dense slurry is 20%, and disk mill gap is 200 μm, and number of processes is 100 times.
(2) C2 in the nano-cellulose for using sodium periodate oxidation step (1) to prepare in glucopyranose structural unit,
The position C3 generates the cellulose with 2,3- dialdehyde based structures.Sodium periodate oxidation condition are as follows: be added in every gram of nano-cellulose
Sodium metaperiodate 1g is protected from light 3h, mixing speed 500r/min at 80 DEG C.
(3) by step (2) aldocellulose and silver ammino solution react to generate after a period of time under heating environment and receive
The nano-cellulose of rice Argent grain load.Silver mirror reaction condition are as follows: silver ammino solution concentration is 0.5mol/L, aldocellulose and silver
The mass ratio of ammonia solution is 1:10, and temperature is 80 DEG C, reacts 5min.
(4) nano-cellulose by the nano-Ag particles load in step (3) is added into poly- third according to certain mass ratio
Alkene nitrile spinning solution, wet spinning, the polyacrylonitrile that sustained-release antibacterial is obtained after drawing-off, washing and drying are fine after mixing
Dimension.The nano-cellulose of nano-Ag particles load and the mass ratio of polyacrylonitrile are 1:500, with the stirring speed of 1000r/min
Degree stirring 5h is uniformly mixed, and draft ratio is 30 times, drying temperature is 30 DEG C.
It is tested by omnipotent mechanical stretch machine and antibacterial tests, the tensile strength of the polyacrylonitrile fibre of the present embodiment is
3.5cN/dtex, the antibiotic rate to Escherichia coli and staphylococcus aureus are respectively 73% and 86%.
Embodiment 3
A kind of polyacrylonitrile fibre of sustained-release antibacterial, preparation method are as follows:
(1) it using rice-straw fibre as raw material, is handled with ultra micron pulverizer and obtains nano-cellulose afterwards for several times.Ultra micron mill
Treatment conditions are as follows: dense slurry is 10%, and disk mill gap is -100 μm, and number of processes is 50 times.
(2) C2 in the nano-cellulose for using sodium periodate oxidation step (1) to prepare in glucopyranose structural unit,
The position C3 generates the cellulose with 2,3- dialdehyde based structures.Sodium periodate oxidation condition are as follows: be added in every gram of nano-cellulose
Sodium metaperiodate 2.5g is protected from light 2h, mixing speed 500r/min at 60 DEG C.
(3) by step (2) aldocellulose and silver ammino solution react to generate after a period of time under heating environment and receive
The nano-cellulose of rice Argent grain load.Silver mirror reaction condition are as follows: silver ammino solution concentration be 0.25mol/L, aldocellulose with
The mass ratio of silver ammino solution is 1:200, and temperature is 50 DEG C, reacts 20min.
(4) nano-cellulose by the nano-Ag particles load in step (3) is added into poly- third according to certain mass ratio
Alkene nitrile spinning solution, wet spinning, the polyacrylonitrile that sustained-release antibacterial is obtained after drawing-off, washing and drying are fine after mixing
Dimension.The nano-cellulose of nano-Ag particles load and the mass ratio of polyacrylonitrile are 1:300, with the mixing speed of 500r/min
It stirs 1.5h to be uniformly mixed, draft ratio is 10 times, drying temperature is 100 DEG C.
It is tested by omnipotent mechanical stretch machine and antibacterial tests, the tensile strength of the polyacrylonitrile fibre of the present embodiment is
4.3cN/dtex, the antibiotic rate to Escherichia coli and staphylococcus aureus are respectively 88% and 91%.
Embodiment 4
A kind of polyacrylonitrile fibre of sustained-release antibacterial, preparation method are as follows:
(1) it using Pinus Massoniana Fibers as raw material, is handled with ultra micron pulverizer and obtains nano-cellulose afterwards for several times.Ultra micron disk
Grind treatment conditions are as follows: dense slurry is 5%, and disk mill gap is -30 μm, and number of processes is 70 times.
(2) C2 in the nano-cellulose for using sodium periodate oxidation step (1) to prepare in glucopyranose structural unit,
The position C3 generates the cellulose with 2,3- dialdehyde based structures.Sodium periodate oxidation condition are as follows: be added in every gram of nano-cellulose
Sodium metaperiodate 2g is protected from light 2h, mixing speed 500r/min at 70 DEG C.
(3) by step (2) aldocellulose and silver ammino solution react to generate after a period of time under heating environment and receive
The nano-cellulose of rice Argent grain load.Silver mirror reaction condition are as follows: silver ammino solution concentration is 0.3mol/L, aldocellulose and silver
The mass ratio of ammonia solution is 1:20, and temperature is 70 DEG C, reacts 30min.
(4) nano-cellulose by the nano-Ag particles load in step (3) is added into poly- third according to certain mass ratio
Alkene nitrile spinning solution, wet spinning, the polyacrylonitrile that sustained-release antibacterial is obtained after drawing-off, washing and drying are fine after mixing
Dimension.The nano-cellulose of nano-Ag particles load and the mass ratio of polyacrylonitrile are 1:100, with the mixing speed of 500r/min
It stirs 3h to be uniformly mixed, draft ratio is 15 times, drying temperature is 110 DEG C.
It is tested by omnipotent mechanical stretch machine and antibacterial tests, the tensile strength of the polyacrylonitrile fibre of the present embodiment is
5.8cN/dtex, the antibiotic rate to Escherichia coli and staphylococcus aureus are respectively 98% and 99%.
Comparative example: virgin pp nitrile fiber comparative example
Virgin pp nitrile fiber the preparation method is as follows:
By polyacrylonitrile spinning solution wet spinning after mixing, through drawing-off, washing and it is dry after obtain polyacrylonitrile
Fiber.200r/min mixing 5h, draft ratio is 15 times, drying temperature is 110 DEG C.
It is tested by omnipotent mechanical stretch machine, the tensile strength of the polyacrylonitrile fibre of this comparative example is 2.1cN/dtex,
Antibiotic rate to Escherichia coli and staphylococcus aureus is respectively 42% and 35%.
The polyacrylonitrile fibre testing result of the sustained-release antibacterial of the different embodiments of table 1
Table 1 lists the polyacrylonitrile fibre testing result of the sustained-release antibacterial prepared in different embodiments, it can be seen that with
The addition of silver-carrying nano fiber, not only increase the tensile strength of polyacrylonitrile fibre, and antibacterial ability has and obviously mentions
It is high.SEM detection is carried out to the polyacrylonitrile fibre of 4 products therefrom sustained-release antibacterial of virgin pp nitrile fiber and embodiment, such as Fig. 2 institute
Show, can be clearly seen that the nano-Ag particles being evenly distributed in the plane of disruption SEM figure of the polyacrylonitrile fibre of sustained-release antibacterial
In the presence of, and the plane of disruption is more neat, achievees the purpose that reinforced polypropylene nitrile fiber.During the preparation process, C2 in nano-cellulose,
The hydroxyl of the position C3 is aldehyde radical through periodate selective paraffin oxidation, and then is converted into carboxyl during silver mirror reaction, provides life
At the indispensable active site of nano silver, the slow-release capability of silver ion is improved.The polyacrylonitrile of sustained-release antibacterial of the present invention
Fiber not only has good anti-microbial property, and tensile strength is greatly improved, and can be applied to anti-biotic material, flat poly-
The various fields such as spinning materials and textile such as Dralon, high modulus polypropylene nitrile fiber, rub resistance acrylic fiber.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of the polyacrylonitrile fibre of sustained-release antibacterial, it is characterised in that include the following steps:
(1) it using plant fiber as raw material, is handled with ultra micron pulverizer and obtains nano-cellulose afterwards for several times；
(2) with the C2 and C3 in the nano-cellulose of periodate oxidation step (1) preparation in glucopyranose structural unit
Position generates the cellulose with 2,3- dialdehyde based structures；
(3) by step (2) with 2,3- dialdehyde based structures cellulose and silver ammino solution one section is reacted under heating environment
The nano-cellulose of nano-Ag particles load is generated after time；
(4) nano-cellulose by the nano-Ag particles load in step (3) is added into polyacrylonitrile according to certain mass ratio
Spinning solution, wet spinning, obtains the polyacrylonitrile fibre of sustained-release antibacterial after drawing-off, washing and drying after mixing.
2. the preparation method of the polyacrylonitrile fibre of sustained-release antibacterial according to claim 1, it is characterised in that: in step (1)
The plant fiber is lumber fibre or/and non-wood-fiber, and the lumber fibre is that aspen fibers by using silicon, Eucalyptus Fibers and pine are fine
At least one of dimension, the non-wood-fiber are that rice-straw fibre, straw fiber, reed fiber, cornstalk fibers and bamboo are fine
At least one of dimension.
3. the preparation method of the polyacrylonitrile fibre of sustained-release antibacterial according to claim 1, it is characterised in that: step (1) institute
The ultra micron pulverizer treatment conditions stated are as follows: disk mill gap is -100~200 μm, and number of processes is 10~100 times.
4. the preparation method of the polyacrylonitrile fibre of sustained-release antibacterial according to claim 1, it is characterised in that: step (2)
Periodate oxidation condition are as follows: 1~5g of periodate is added in every gram of nano-cellulose, it is protected from light 1 at 40~80 DEG C~
3h, mixing speed are 100~1000r/min.
5. the preparation method of the polyacrylonitrile fibre of sustained-release antibacterial according to claim 1, it is characterised in that: step (3) institute
Stating silver ammino solution concentration is 0.01~0.5mol/L, and the mass ratio of cellulose and silver ammino solution with 2,3- dialdehyde based structures is
1:(10~500)；Silver-colored ammonia heats reaction condition are as follows: temperature is 40~80 DEG C, reacts 5~60min.
6. the preparation method of the polyacrylonitrile fibre of sustained-release antibacterial according to claim 2, it is characterised in that: in step (4)
The mass ratio of polyacrylonitrile is 1:(1~1000 in the nano-cellulose and spinning solution of nano-Ag particles load), with 100~
The mixing speed of 1000r/min stirs 1~5h and is uniformly mixed；Draft ratio is 1~30 times, drying temperature is 30~130 DEG C.
7. delaying made from a kind of preparation method of the polyacrylonitrile fibre as sustained-release antibacterial as claimed in any one of claims 1 to 6
Release the polyacrylonitrile fibre of antibacterial.
8. the polyacrylonitrile fibre of sustained-release antibacterial as claimed in claim 7 is in anti-biotic material, flat polyacrylonitrile fibre, high-modulus
Application in polyacrylonitrile fibre and rub resistance acrylic fiber field.
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| CN114213559A (en) * | 2021-12-06 | 2022-03-22 | 扬州大学 | Selenized polyacrylonitrile antibacterial material |
| CN115555577A (en) * | 2022-10-17 | 2023-01-03 | 华南理工大学 | High-stability silver nanocluster fluorescent probe and preparation method and application thereof |
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