CN106283404B - The method for preparing nano silver blending native cellulose melt-blown nonwoven fabric - Google Patents
The method for preparing nano silver blending native cellulose melt-blown nonwoven fabric Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The present invention relates to a kind of methods for preparing nano silver blending native cellulose and being meltblown nonwoven fabric, are with polyvinyl alcohol（PVA）The protective agent that gel state is made in pure water is added in powder, adds silver nitrate（AgNO3）And sodium borohydride（NaBH4）The polyvinyl alcohol protective agent is set to form nano silver colloidal sol with silver nitrate reduction; then; wood pulp is added in the nano silver colloidal sol to mix in the cellulose slurries of dissolving with oxidation methyl beautiful jade; the mucus (dope) of nano silver native cellulose is formed after removing moisture removal; mucus is squeezed out to form long fibre element tow by (meltblown) from mouth is spun in a manner of being meltblown again; after finally the programs such as rolling, drying and batching via regeneration, washing, liquid drugs injection, you being made, there is antistatic and antibacterial functions nano silver native cellulose to be meltblown nonwoven fabric.
Description
Technical field
The present invention relates to a kind of methods for preparing nano silver blending native cellulose and being meltblown nonwoven fabric, are to belong to environmentally protective
Processing procedure manufactures the technical field of natural fiber nonwoven fabric, is pure water to be added with polyvinyl alcohol (PVA) powder gel state is made
Poly-vinyl alcohol solution, and silver nitrate (AgNO is added3) solution be metal salt precursor body, add sodium borohydride (NaBH4), make this
Poly-vinyl alcohol solution restores to form nano silver colloidal sol, and then, nano silver colloidal sol addition wood pulp is mutually mixed with methyl morpholine oxide
In the cellulose slurries for closing dissolving, the mucus (dope) of nano silver native cellulose is formed after removing moisture removal, then with melt-blown side
Mucus is squeezed out to form long fibre element tow by formula (meltblown) from mouth is spun, and is finally rolled, is done via regeneration, washing, liquid drugs injection
It is dry and after the programs such as batching, you being made, there is antistatic and antibacterial functions nano silver native cellulose to be meltblown nonwoven fabric.
Background technology
Nano silver colloidal sol and high polymer fibre are mixed to made chemical fibre technology at present, disclosed as Chinese special
Sharp application number 200410062799.3,200510070895.7,201010230063.8,201010285121.7 and
201310523647.8 etc., have effects that antibacterial by the chemical fibre and the nonwoven fabric with antibacterial functions can be made,
However, when the nonwoven fabric made by aforementioned high polymer fibre becomes waste after use, due to cannot be decomposed by natural environment
Huge impact and burden are generated to environment, while can also discharge harmful substance in processing procedure, in addition, aforementioned each processing procedure is made
The nonwoven fabric of nano silver chemical fibre its antibiotic effect degree differs, be unable to reach the exact requirements using end.
Therefore, such as the how not native cellulose fibre of present environmental risks, and under the process conditions accurately controlled
There is antistatic and antibacterial functions nano silver native cellulose nonwoven fabric to reach to prepare, just seem it is anxious for urgently with needs.
Invention content
The main object of the present invention is providing a kind of method for preparing nano silver blending native cellulose and being meltblown nonwoven fabric,
Step includes：A, it stirs polyvinyl alcohol (Polyvinyl Alcohol, abbreviation PVA) powder addition pure water to form gel state
Poly-vinyl alcohol solution, and silver nitrate (AgNO is added3) solution be metal salt precursor body；B, sodium borohydride (NaBH is added4) Yu Juyi
In enol gel solution, it is stirred titration reduction and forms nano silver colloidal sol；C, wood pulp and oxidation first is added in nano silver colloidal sol
In the slurries of Ji Malin (N-methylmorpholine N-oxide, abbreviation NMMO) mixed dissolution；It first cuts raw material of wood pulp
It is broken and with oxidation methyl agate beautiful jade, stabilization agent jointly put into expansion dissolving tank in be mixed, slot domestic demand heated at constant temperature is in 60~80
Between DEG C, and vacuum condensation equipment of arranging in pairs or groups is removed water；D, the moisture formation spinning of slurries is blended in removal nano silver native cellulose
Silk mucus (dope)；It is that extra moisture content is evaporated using Vacuum film evaporation device (Thin Film Evaporator, TFE),
Vacuum degree in the Vacuum film evaporation device is heated between -9.39*10^4~-9.26*10^4Pa, and with 80 DEG C~130 DEG C,
Moisture is excluded in 5~10 minutes to 5%~15%, you can by cellulose dissolution at the mucus of spinning；E, in a manner of being meltblown
(meltblown) mucus is squeezed out to form long fibre element tow from mouth is spun；It is with metering pump pressure-increasing unit spinning mucus,
Enter in manifold after continuous filter (CPF) filtering, deaeration, is persistently poured by hot-air and spin mouth and arranged around mouth from spinning
The airflow function gone out forces mucus to be meltblown from spinning mouth and squeezes out external formation long fibre element tow；F, spraying water mist makes length
Cellulose tow enters solidification regeneration and washing in solidification liquid；And g, the long fibre element tow after solidification liquid regeneration washing are being held
It connects and mutually stacks into the nonwoven fabric of net form on the net, then after sequentially being rolled through liquid drugs injection, drying and batch program, it is natural to obtain nano silver
Cellulose is meltblown nonwoven fabric.By the particle size and concentration that can control the nano silver colloidal sol in processing procedure so that prepare nanometer
The antibiotic effect of silver-colored native cellulose melt-blown nonwoven fabric, in addition to it can meet requirement of the different consumption terminals to antibiotic effect degree,
Its effect is farther be more than it is general sold on the market to be surface-treated or add the nonwoven fabric of antibacterial, and it is using again can quilt after abandoning
Natural decomposition, and as the environmentally friendly nonwoven fabric of harmless natural environment.
Another mesh of the present invention is to provide a kind of method for preparing nano silver blending native cellulose and being meltblown nonwoven fabric, by
By the particle size and concentration that can control the nano silver colloidal sol in its processing procedure so that prepare the melt-blown of nano silver native cellulose not
And it can be by certainly after antistatic effect of woven fabric can meet requirement of the different consumption terminals to antistatic degree, and its use abandons
So decompose, and as the environmentally friendly nonwoven fabric of harmless natural environment.
The technical scheme is that：A method of preparing nano silver blending native cellulose melt-blown nonwoven fabric, step
Suddenly include：A, polyvinyl alcohol powder addition pure water is stirred to the poly-vinyl alcohol solution to form gel state, and silver nitrate solution is added
For metal salt precursor body；Wherein, the additive amount of the polyvinyl alcohol is 5-12wt%, and uses basicity for 86~89mole%'s
Part alkalization type polyvinyl alcohol powder, molecular weight are 14700~98000, which is to be dissolved in silver nitrate crystal
It is formulated in pure water；B, be added sodium borohydride in polyvinyl alcohol gel solution, be stirred titration reduction form nano silver
Colloidal sol；Wherein, which is with mole number than 1:4~1:8 carry out reductometry, and titration speed is 5~15ml per minute,
Stirring frequency is 10~20 minutes in 200rpm, the reaction time for titrating completion, obtained nano silver colloidal sol a concentration of 500~
20,000ppm, nano-Ag particles grain size is 10~150nm；C, nano silver colloidal sol addition wood pulp is mixed with oxidation methyl agate beautiful jade
In the slurries of dissolving；Raw material of wood pulp is first shredded and is put into jointly with oxidation methyl agate beautiful jade, stabilization agent in expansion dissolving tank and mixed by it
Stirring is closed, slot domestic demand heated at constant temperature is between 60~80 DEG C, and vacuum condensation equipment of arranging in pairs or groups is removed water, in the expansion dissolving tank
Vacuum degree between -9.33*10^4Pa, wherein in the slurries of the mixed dissolution ratio of nano silver colloidal sol between 5~
30wt%, the concentration of nano silver particles is between 100~5000ppm；D, the water of slurries is blended with native cellulose for removal nano silver
Divide and forms spinning mucus；It is to evaporate extra moisture content using Vacuum film evaporation device, the vacuum in the Vacuum film evaporation device
Degree is heated between -9.39*10^4~-9.26*10^4Pa, and with 80 DEG C~130 DEG C, exclude in 5 minutes moisture to 5%~
15%, you can by cellulose dissolution at the mucus of spinning；Wherein, each composition proportion is in mucus：Water accounts for 9%~18%,
Oxidation methyl agate beautiful jade accounts for 75%~87%, and cellulose accounts for 6%~11%；E, in a manner of being meltblown (meltblown) by mucus from spinning
Mouth squeezes out to form long fibre element tow；It is with metering pump pressure-increasing unit spinning mucus, through continuous filter filtering, deaeration
Enter in manifold afterwards, is persistently poured by hot-air and spin mouth and from the airflow function being discharged around mouth is spun, force mucus from spinning
It is meltblown in mouthful and squeezes out external formation long fibre element tow；F, spraying water mist makes long fibre element tow enter in solidification liquid to solidify
Regeneration and washing；Wherein, solidification liquid concentration remaining oxidation methyl agate beautiful jade quantity of solvent after 2.5%~7.0%, washing is less than
0.1%, polyvinyl alcohol residual quantity is less than 0.3%；And g, the long fibre element tow after solidification liquid regeneration washing are in bearing net
The nonwoven fabric of net form is mutually stacked into, then after sequentially being rolled through liquid drugs injection, drying and batch program, obtains nano silver native cellulose
It is meltblown nonwoven fabric.
Beneficial effects of the present invention are：A kind of method preparing nano silver blending native cellulose melt-blown nonwoven fabric is provided,
By the particle size and concentration that can control the nano silver colloidal sol in its processing procedure so that prepare the melt-blown of nano silver native cellulose
The antibiotic effect of nonwoven fabric, in addition to it can meet requirement of the different consumption terminals to antibiotic effect degree, effect is farther more than one
As sold on the market to be surface-treated or add the nonwoven fabric of antibacterial, and it is using again can be by natural decomposition after abandoning, and becomes
The environmentally friendly nonwoven fabric of harmless natural environment.In addition, by the particle size and concentration that can control the nano silver colloidal sol in its processing procedure,
So that preparing antistatic effect of nano silver native cellulose melt-blown nonwoven fabric, different consumption terminals can be met to antistatic journey
The requirement of degree, and again can be by natural decomposition after its use discarding, and become the environmentally friendly nonwoven fabric of harmless natural environment.
Description of the drawings
Fig. 1 is the manufacturing process block diagram of the present invention.
Fig. 2 is the chemical structural drawing of polyvinyl alcohol used herein (Polyvinyl Alcohol, abbreviation PVA).
Fig. 3 is oxidation methyl agate beautiful jade solvent used herein (N-methylmorpholine N-oxide, abbreviation
NMMO chemical structural drawing).
Fig. 4 is the chemical structural drawing of wood pulp cellulose used herein (Cellulose).
Fig. 5 is the grain size distribution of 1000ppm nano silver colloidal sols in the present invention.
Fig. 6 is electron microscope (TEM) figure that 1000ppm nano silver colloidal sols dilute after 100 times in the present invention.
Specific label is as follows in figure：
Nothing
Specific implementation mode
For the production process and effect further illustrated the present invention, Zi Zuo is to illustrate and each test examples are described in detail such as
Afterwards：
Shown in please referring to Fig.1 to Fig.4, the method that the present invention prepares nano silver blending native cellulose melt-blown nonwoven fabric,
Step includes：
A, it stirs polyvinyl alcohol (Polyvinyl Alcohol, abbreviation PVA) powder addition pure water to form the poly- of gel state
Glycohol solution, and silver nitrate (AgNO is added3) solution be metal salt precursor body；Wherein, the additive amount of the polyvinyl alcohol is 5-
12wt%, and use basicity for the part alkalization type polyvinyl alcohol powder of 86~89mole%, molecular weight is 14700~
98000, chemical structural drawing is as shown in Fig. 2, its and cold soluble low with the degree of polymerization is in the characteristic of water, and the concentration added can be really
The generation of real cladding and protection silver particles；The silver nitrate solution is that silver nitrate crystal is dissolved in pure water to be formulated；
B, sodium borohydride (NaBH is added4) in polyvinyl alcohol gel solution, be stirred titration reduction form nano silver
Colloidal sol；Wherein, which is with mole number than 1:4~1:8 carry out reductometry, and titration speed is 5~15ml per minute,
Stirring frequency is 10~20 minutes in 200rpm, the reaction time for titrating completion, obtained nano silver colloidal sol a concentration of 500~
20,000ppm, nano-Ag particles grain size is 10~150nm；
C, wood pulp and oxidation methyl agate beautiful jade (N-methylmorpholine N-oxide, abbreviation is added in nano silver colloidal sol
NMMO) in the slurries of mixed dissolution；Its first by raw material of wood pulp shred and with oxidation methyl agate beautiful jade (chemical structural drawing such as Fig. 3 institutes
Show), stabilization agent put into expansion dissolving tank and be mixed jointly, slot domestic demand heated at constant temperature is between 60~80 DEG C, and it is true to arrange in pairs or groups
Empty condensing plant is removed water, and the vacuum degree in the expansion dissolving tank is between -9.33*10^4Pa, wherein the raw material of wood pulp is
Long fibre wood pulp (soft wood) mixes with short fine wood pulp (hard wood), and the weight ratio of both celluloses is 0：100~
100：0, the wood pulp degree of polymerization used is 500~1200, and alpha-cellulose content is 85% or more, chemical structural drawing such as Fig. 4 institutes
Show, and in the mixed dissolution slurries ratio of nano silver colloidal sol between 5~35wt%, the concentration of nano silver particles between 100~
5000ppm；
D, the moisture formation spinning mucus (dope) of slurries is blended with native cellulose for removal nano silver；It is to use vacuum
Thin film evaporator (Thin Film Evaporator, TFE) evaporates extra moisture content, the vacuum degree in the Vacuum film evaporation device
Heated between -9.39*10^4~-9.26*10^4Pa, and with 80 DEG C~130 DEG C, exclude in 5~10 minutes moisture to 5%~
15%, you can by cellulose dissolution at the mucus of spinning；It is good due to having between two system of native cellulose and polyvinyl alcohol
The characteristics of compatibility, can closely combine and run through each other both in the Blending Processes of sizing mixing of step c, then penetrate machine
The shear action of tool stirring can form the structure of approximate continuous phase, and the homogenization degree of two-phase is higher, the stability of spinning mucus
It is opposite to improve, and can ensure that nano-Ag particles are evenly dispersed in spinning mucus；Wherein, each composition proportion in mucus
For：Water (H2O 9%~18%) is accounted for, oxidation methyl agate beautiful jade (NMMO) accounts for 75%~87%, and cellulose (cellulose) accounts for 6%~
11%；
E, mucus is squeezed out to form long fibre element tow by (meltblown) from mouth is spun in a manner of being meltblown；It is in terms of
Amount pump pressure-increasing unit spinning mucus, enters in manifold after continuous filter (CPF) filtering, deaeration, continues by hot-air
It pours into and spins mouth and from the airflow function being discharged around mouth is spun, force mucus to be meltblown from spinning mouth and squeeze out external formation long fibre
Plain tow；
F, spraying water mist makes long fibre element tow enter solidification regeneration and washing in solidification liquid；Wherein, solidification liquid concentration is situated between
Remaining oxidation methyl agate beautiful jade quantity of solvent is less than 0.1% after 2.5%~7.0%, washing, and polyvinyl alcohol residual quantity is less than
0.3%；And
G, the long fibre element tow after solidification liquid regeneration washing mutually stacks into the nonwoven fabric of net form in bearing net, then
After sequentially being rolled through liquid drugs injection, drying and batch program, nano silver native cellulose melt-blown nonwoven fabric is obtained.
Wherein, regeneration and the polyvinyl alcohol in mixed solution after washing in step f, can penetrate the mode one combined with aqueous
And dissolve out and must be pocessed, it is to import the mixed solution in chromatography tank, and sequentially add saltcake 100g/L (Na2SO4)、
Borax 16.7g/L (Na2B4O7.10H2O) two kinds of quantitative proportionings add a small amount of sodium carbonate (Na2CO3) adjusted as pH
Agent so that polyvinyl alcohol is agglomerated, gelatinization is precipitated, and mutually can be separated out with oxidation methyl agate beautiful jade solvent via after filtering,
It can be to avoid influencing the recycling and utilization of oxidation methyl agate beautiful jade solvent.
The oxidation methyl agate beautiful jade solvent for regenerating in another step f and being disengaged after washing, because high number must also be subject to whole
Recycling come fully recycles, recycle the step of include：
A. first time filtering is first carried out with the PP filter cores of 1~20 μ；
B. it will inject in flocculation tank filtered solvent for the first time, the dosage of the additive of flocculant and its cooperation is
1.5mg/L, 1 hour processing time, the colloidal impurity in solvent is poly- attached by the effect generation of flocculant, and non-solubility is miscellaneous in solution
Matter can form the flocculate of high state of aggregation, and measuring big flocculate can start to settle, and then penetrate strainer barrier discharge again；
C. at flocks after solvent be passed directly into ion-exchange purification system, through charging property anions and canons
Absorption, conjugation, can detach the foreign pigment in solution, and reinforce the purifying of solvent, the pH ranges dimension during the processing
It is held in 8~9；
D. second is carried out to solvent after purification again with ultrafilter (UF) and reverse osmosis (RO) filter to filter；
And
E. finally second of filtered low-concentration oxidizing methyl agate beautiful jade solvent (3.0%~6.0%) is carried out at concentration
Reason, adopt multi-stage evaporation tank systems and recycled, during cycle oxidation methyl agate beautiful jade solvent will gradually purify until
50.0%~78.0% output and reach recycling, and can by it again put into return production line use, can by aforementioned recovery process
Make the rate of recovery of oxidation methyl agate beautiful jade up to 99.5% or more.
It is carrying out completing every test examples and illustrating as after further to prove the features of the present invention and implementing effect：
Embodiment one：
5.0g part alkalization type polyvinyl alcohol is added in 95.0g pure water, the 2 hours poly- second up to 5wt% is persistently stirred
Enolate solution is dissolved in pure water with suitable silver nitrate crystal and is configured to 0.1N silver nitrate solution 0.5ml, and polyvinyl alcohol is added
Stirred evenly in gel solution, then with the sodium borohydride of 0.2N with the speed of 5ml per minute carry out reductometry to get
The nano silver colloidal sol of 1000ppm, polyvinyl alcohol gel can become yellowish-brown again with translucent gradual flavescence in reduction process, up to drop
Determine to should be light brown when terminal.
Nano silver colloidal sol sample obtained as above is subjected to particle diameter distribution, as shown in Figure 5.And it will be after 100 times of sample dilution
Electron microscope (TEM) image authentication is carried out, as shown in Figure 6.
By the result of quantitative analysis in Fig. 5 it can be seen that, its particle diameter distribution of the nano silver gel of 1000ppm in 7~115nm,
Average Particle Diameters are 23.5nm.It is also shown again by the TEM micrograph picture of Fig. 6, nanoscale can be restored really and be less than
The silver particles of 100nm.
Embodiment two：
The wood pulp that the degree of polymerization is 650 is mixed into cellulose slurries with oxidation methyl agate beautiful jade solvent, then adds 5~35wt%
Nano silver colloidal sol blended；Wherein a concentration of 100~5000ppm of nano silver particles is evaporated with Vacuum film evaporation device
Extra moisture content is heated with 80 DEG C~130 DEG C, moisture is excluded in 5 minutes to 5%~13%, you can by cellulose dissolution at spinning
Silk mucus (dope), spinning mucus form table such as【Table one】It is shown, then in a manner of being meltblown (meltblown) by mucus with metering pump
Pressure-increasing unit through continuous filter (CPF) filtering, enters in manifold after deaeration, persistently poured by hot-air spin mouth and from
The airflow function being discharged around mouth is spun, forces mucus to be meltblown from spinning mouth and squeezes out external formation long fibre element tow, then into
After entering solidification regeneration in solidification liquid and washing, which can mutually stack into the nonwoven fabric of net form in bearing net,
After finally sequentially being rolled through liquid drugs injection, drying and batch program, nano silver native cellulose melt-blown nonwoven fabric is obtained, it is obtained as above
Nonwoven fabric sample is such as【Table one】Shown in middle sample number into spectrum 1~11.
Embodiment three：
Wood pulp and oxidation methyl agate beautiful jade solvent that the degree of polymerization is 1050 are mixed into cellulose slurries, then afterwards addition 5~
The nano silver colloidal sol of 35wt% is blended；Wherein a concentration of 100~5000ppm of nano silver particles, with Vacuum film evaporation
Device evaporates extra moisture content, is heated with 80 DEG C~130 DEG C, moisture is excluded in 5 minutes to 5%~13%, you can cellulose is molten
Solution forms table such as at spinning mucus (dope), spinning mucus【Table one】It is shown, then in a manner of being meltblown (meltblown) by mucus with
Metering pump pressure-increasing unit enters in manifold after continuous filter (CPF) filtering, deaeration, spinning is persistently poured by hot-air
Mouth and the airflow function being discharged around spinning mouth force mucus to be meltblown from spinning mouth and squeeze out external formation long fibre element silk
Beam, after entering back into solidification regeneration in solidification liquid and washing, which can mutually stack into net form in bearing net
Nonwoven fabric after finally sequentially being rolled through liquid drugs injection, drying and batch program, obtains nano silver native cellulose melt-blown nonwoven fabric, with
The nonwoven fabric sample of upper gained is such as【Table one】Shown in middle sample number into spectrum 12~22.
【Table one】：Each sample spinning solution forms table
Example IV (assessments of antibacterial functions)：
The assessment of antibacterial functions uses staphylococcus aureus (ATCC 6538P) and pneumobacillus (ATCC 4352) to survey
Try strain.The silver particles of nanosizing are positively charged, when nano silver particles are in free state, can be connect with electronegative bacterial cell membrane
It touches, the two forms the structure of a dehydrogenase-SAg after be combineding with each other.Its cell can be destroyed into endobacillary nano silver to live
Property, damage DNA of bacteria and interrupt cellular signal transduction, further suppress bacterial growth；Thalline after nano silver effect simultaneously
Cell membrane can be gradually weak or even perforates, and leads to a large amount of reduced sugar, protein and K+From thalline internal leakage, film potential
It is consumed totally with ATP, makes bacterium that can not breathe, be metabolized and breed, until dead.
The examination of antibiotic property will be carried out to the native cellulose melt-blown nonwoven fabric containing nano silver particles prepared by the present invention
It tests, tests whether it has antibiotic property.
【Table two】、【Table three】The test result of nonwoven fabric antibacterial functions is meltblown for native cellulose containing nano silver particles.This
Test method is JIS L1902-1998 sizing techniques, and test strain is staphylococcus aureus (ATCC 6538P) and pneumonia bar
Bacterium (ATCC 4352).Wherein, it plants bacteria concentration and indicates that experiment is effective in 1.0 ± 0.3 E+5 (bacterium number/milliliter), Ma=is undressed
Sample washes away rear bacterium number for 0 hour immediately, bacterium number after sample culture in 18~24 hours that Mb=is undressed, Mc=processed samples 18~24
Bacterium number after hour culture；Bacterium growth activity value=logMb-logMa, bacterium growth activity value>1.5 indicate that experiment is effective, suppression
Bacterium value=logMb-logMc, sterilizing value=logMa-logMc；Consultation is evaluated according to the Japanese new function of fibre
(JAFET) antibacterial standard, antibacterial value, which is more than 2.2 expression test samples, has fungistatic effect, sterilizing value to be more than 0 and indicate test sample
There is bactericidal effect；1.3E+4 indicates 13000, and so on.
By【Table two】And【Table three】It is found that not via the melt-blown of native cellulose containing nano silver particles prepared by the present invention
Woven fabric, itself has quite good fungistatic effect and bactericidal effect for staphylococcus aureus and pneumobacillus.
The antibacterial tests result of each sample is such as【Table two】、【Table three】It is shown.
【Table two】：Native cellulose containing nano silver particles is meltblown the antibacterial functions experiment of nonwoven fabric
This test method is JIS L1902-1998 sizing techniques, and test strain is staphylococcus aureus (ATCC
6538P)。
【Table three】：Native cellulose containing nano silver particles is meltblown the antibacterial functions experiment of nonwoven fabric
This test method is JIS L1902-1998 sizing techniques, and test strain is pneumobacillus (ATCC 4352).
Embodiment five (the antibacterial functions assessment after washing 10 times)：
Each sample is cleaned 45 minutes 10 times in 70 DEG C of hot water with the laundry paks of 5g/L, gained each sample is resisted
Bacterium is tested, and the result of gained is such as【Table four】It is shown.
【Table four】：Native cellulose containing nano silver particles is meltblown nonwoven fabric antibacterial functions after washing 10 times and tests
This test method is JIS L1902-1998 sizing techniques, and test strain is pneumobacillus (ATCC 4352).
By【Table two】、【Table three】Cellulose containing nano silver particles is meltblown nonwoven fabric antibacterial functions test result and shows, this
The concentration of the nano silver particles added in the cellulose melt-blown nonwoven fabric of invention has effects that sterilization up to 100ppm or more,
If addition concentration shows its excellent biocidal property more than 1500ppm.By【Table two】、【Table three】Example it is all provable, this
The effect of cellulose melt-blown nonwoven fabric containing nano silver particles of invention can reach antibacterial really, and its antibacterial efficacy is with nano silver
The increase of particle concentration and promoted.
Separately by【Table four】Native cellulose containing nano silver particles is meltblown nonwoven fabric antibacterial functions experiment knot after washing 10 times
Fruit shows that native cellulose containing nano silver particles of the invention is meltblown nonwoven fabric after 10 hot water and detergent treatment, no
The antibacterial functions effect of woven fabric still maintains 90% or more before not washing originally, and what thus result display was of the invention contains nano silver
It is an antibacterial cellulose nonwoven fabric with long-acting type that particle native cellulose, which is meltblown nonwoven fabric, and effect is far more than general market
On sell to be surface-treated or add the nonwoven fabric of antiseptic.
Embodiment six (anti-static function assessment)：
Anti-static function detection is according to antistatic textile standard FTTS-FA-009, and the specification of reference AATCC76 is with same
The heart is justified electrode surface resistance and is carried out, and the sheet resistance value of each sample is tested, and it is molten to use evaluation native cellulose containing nano silver particles
Spray antistatic effect of nonwoven fabric.
【Table five】：Native cellulose containing nano silver particles is meltblown the experiment of nonwoven fabric anti-static function
By【Table five】The results show that native cellulose containing nano silver particles melt-blown nonwoven fabric except addition content be less than
It is the specification grade of grade 2 outside the sample of 100ppm；Indicate that its antistatic effect is " it is good " evaluation, and the table of fiber
Surface resistance value (resistance) can also be promoted with the increase of added nano silver particles concentration.In addition, prepared by the present invention
The melt-blown nonwoven fabric of native cellulose containing nano silver particles gone out, antistatic property are not also knitted far above what is generally sold on the market
Cloth.
In conclusion the native cellulose containing nano silver particles prepared by the present invention is meltblown nonwoven fabric, have apparent anti-
The effect of bacterium function, therefore be conducive to improve the value and application of textile, and consumption terminal can be met, antimicrobial levels are wanted
It asks, can effectively inhibit microorganism (comprising bacterium, mould or true by the native cellulose containing nano silver particles melt-blown nonwoven fabric
Bacterium) breeding and growth, or even kill germ, while may achieve and avoid the cross-infection of bacterium, controlling the propagation of disease, and have
Conducive to promotion health, cleaning, comfortable life.In addition, it is more because of the antistatic effect having had, therefore this contains nano silver particles day
Right cellulose is meltblown nonwoven fabric, the electrocution conditions occurred when also effectively winter can be avoided to wear off clothing, thus it is quiet to reach reduction
The tired negative effect to caused by blood circulation of human body, immune and nervous system of electrodeposition.It is really a quite practical innovation hair
It is bright, patent application condition should be met, whence is filed an application in accordance with the law.
Claims (4)
1. a kind of method preparing nano silver blending native cellulose melt-blown nonwoven fabric, which is characterized in that step includes：
A, polyvinyl alcohol powder addition pure water is stirred to the poly-vinyl alcohol solution to form gel state, and it is gold that silver nitrate solution, which is added,
Belong to salt precursor body；Wherein, the additive amount of the polyvinyl alcohol is 5-12wt%, and uses basicity for the part of 86~89mole%
Alkalization type polyvinyl alcohol powder, molecular weight are 14700~98000, which is that silver nitrate crystal is dissolved in pure water
In be formulated；
B, be added sodium borohydride in polyvinyl alcohol gel solution, be stirred titration reduction form nano silver colloidal sol；Wherein, should
Sodium borohydride is with mole ratio 1:4~1:8 carry out reductometry, and titration speed is 5~15ml per minute, and stirring frequency exists
200rpm, the reaction time for titrating completion is 10~20 minutes, and obtained nano silver colloidal sol a concentration of 500~20,000ppm receive
Rice Argent grain grain size is 10~150nm；
C, nano silver colloidal sol is added in the slurries of wood pulp and oxidation methyl agate beautiful jade mixed dissolution；It first shreds raw material of wood pulp simultaneously
With oxidation methyl agate beautiful jade, stabilization agent jointly put into expansion dissolving tank in be mixed, slot domestic demand heated at constant temperature in 60~80 DEG C it
Between, and vacuum condensation equipment of arranging in pairs or groups is removed water, the vacuum degree in the expansion dissolving tank is -9.33*10^4Pa, wherein this is mixed
The ratio of nano silver colloidal sol in the slurries of dissolving is closed between 5~30wt%, the concentration of nano silver particles is between 100~5000ppm；
D, the moisture formation spinning mucus of slurries is blended with native cellulose for removal nano silver；It is to use Vacuum film evaporation device
Evaporate extra moisture, the vacuum degree in the Vacuum film evaporation device between -9.39*10^4~-9.26*10^4Pa, and with
80 DEG C~130 DEG C heating exclude moisture to 5%~15%, you can by cellulose dissolution at the mucus of spinning in 5 minutes；Wherein,
Each ingredient proportion is in mucus：Water accounts for 9%~18%, and oxidation methyl agate beautiful jade accounts for 75%~87%, and cellulose accounts for 6%~
11%；
E, mucus is squeezed out to form long fibre element tow from mouth is spun in a manner of melt-blown；It is with metering pump pressure-increasing unit spinning
Mucus enters after continuous filter filtering, deaeration in manifold, is persistently poured by hot-air and spins mouth and arranged around mouth from spinning
The airflow function gone out forces mucus to be meltblown from spinning mouth and squeezes out external formation long fibre element tow；
F, spraying water mist makes long fibre element tow enter solidification regeneration and washing in solidification liquid；Wherein, solidification liquid concentration between
2.5%~7.0%, remaining oxidation methyl agate beautiful jade quantity of solvent is less than 0.1% after washing, and polyvinyl alcohol residual quantity is less than 0.3%；
And
G, the long fibre element tow after solidification liquid regeneration washing mutually stacks into the nonwoven fabric of net form in bearing net, then sequentially
After being rolled through liquid drugs injection, drying and batch program, nano silver native cellulose melt-blown nonwoven fabric is obtained,
Regeneration and the polyvinyl alcohol in mixed solution after washing, are to be conducted into chromatography tank, and sequentially add saltcake in step f
Two kinds of 100g/L, borax 16.7g/L quantitative proportionings, add a small amount of sodium carbonate as pH adjusting agent so that polyvinyl alcohol
It is agglomerated, gelatinization precipitation,
In step f regeneration with wash after the recycling step of oxidation methyl agate beautiful jade solvent that disengages include：
A. first time filtering is first carried out with 1~20 μm of PP filter cores；
B. it will inject in flocculation tank filtered solvent for the first time, the dosage of the additive of flocculant and its cooperation is 1.5mg/
L, 1 hour processing time, the colloidal impurity in solvent is poly- attached by the effect generation of flocculant, and non-solubility impurity can shape in solution
At the flocculate of high state of aggregation, measuring big flocculate can start to settle, and then penetrate strainer barrier discharge again；
C. through flocks, treated that solvent is passed directly into ion-exchange purification system, through charging property anions and canons absorption,
Foreign pigment in solution can be detached, and reinforce the purifying of solvent by conjugation, and the pH ranges during the processing are maintained at 8
~9；
D. second is carried out to solvent after purification again with ultrafiltration and reverse osmosis filter to filter；And
E. second of filtered low-concentration oxidizing methyl agate beautiful jade solvent 3.0%~6.0% is finally subjected to concentration, adopted
It is recycled with multi-stage evaporation tank systems, oxidation methyl agate beautiful jade solvent will be purified gradually until 50.0% during cycle
~78.0% can output reach recycling.
2. a kind of method preparing nano silver blending native cellulose melt-blown nonwoven fabric as described in claim 1, feature exist
In：The raw material of wood pulp is that long fine wood pulp is mixed with short fine wood pulp in step c, and the weight ratio of both celluloses is 0：100~
100：0, the wood pulp degree of polymerization used is 500~1200, and alpha-cellulose content is 85% or more.
3. a kind of method preparing nano silver blending native cellulose melt-blown nonwoven fabric as described in claim 1, feature exist
In：The raw material of wood pulp is long fine wood pulp in step c, and the wood pulp degree of polymerization used is 500~1200, and alpha-cellulose content exists
85% or more.
4. a kind of method preparing nano silver blending native cellulose melt-blown nonwoven fabric as described in claim 1, feature exist
In：The raw material of wood pulp is short fine wood pulp in step c, and the wood pulp degree of polymerization used is 500~1200, and alpha-cellulose content exists
85% or more.
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| CN1936124A (en) * | 2005-09-22 | 2007-03-28 | 河北吉藁化纤有限责任公司 | Silver-containing antibacterial viscose fiber and its preparing method |
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| CN102776594A (en) * | 2012-07-10 | 2012-11-14 | 东华大学 | Cellulose fiber-supported nano silver antibacterial material and preparation method thereof |
| CN103820992A (en) * | 2014-03-07 | 2014-05-28 | 青岛大学 | Preparation method for silver golden regenerated cellulose fiber/silver golden regenerated cellulose fiber fabric |
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| CN1936124A (en) * | 2005-09-22 | 2007-03-28 | 河北吉藁化纤有限责任公司 | Silver-containing antibacterial viscose fiber and its preparing method |
| CN102127841A (en) * | 2010-01-13 | 2011-07-20 | 聚隆纤维股份有限公司 | Production method of cellulose non-woven fabric with functions of mildew proofing, antibiosis and deodorization through wet-type meltbrown |
| CN102776594A (en) * | 2012-07-10 | 2012-11-14 | 东华大学 | Cellulose fiber-supported nano silver antibacterial material and preparation method thereof |
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