CN110079882A - A kind of preparation method of antimicrobial form polypropylene fibre - Google Patents
A kind of preparation method of antimicrobial form polypropylene fibre Download PDFInfo
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- CN110079882A CN110079882A CN201910358349.5A CN201910358349A CN110079882A CN 110079882 A CN110079882 A CN 110079882A CN 201910358349 A CN201910358349 A CN 201910358349A CN 110079882 A CN110079882 A CN 110079882A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to the modified fields of polypropylene fibre, and in particular to a kind of preparation method of antimicrobial form polypropylene fibre.The present invention obtains the silane moiety hydrolytic condensate of chloropropyl containing 3- and dodecyl group using dodecyl trialkoxy silane and 3- chloropropyl the trialkoxy silane hydrolytic condensation in insufficient amount of deionized water, silane moiety hydrolytic condensate reacts with nanometer Tai Ji stone again, obtain dodecyl group and the co-modified nanometer Tai Ji stone of 3- chloropropyl group, 3- chloropropyl group and N therein, quaternization reaction occurs for N- dimethyl alkyl tertiary amine, obtain dodecyl group and the co-modified nanometer Tai Ji stone of quaternary ammonium salt group, it is added in PP GRANULES after melt pelletization and obtains antimicrobial form polypropylene fibre with PP GRANULES melt spinning again.The antimicrobial form polypropylene fibre that the present invention obtains have preferable normal direction far infrared transmissivity, biocidal property and washability, can single textile molding or be made into type with other fiber cospinnings.
Description
Technical field
The present invention relates to the modified fields of polypropylene fibre, and in particular to a kind of preparation method of antimicrobial form polypropylene fibre.
Background technique
As people's living standard is higher and higher, the antimicrobial form of textile, especially personal clothing is required higher.
Quarternary ammonium salt compound can adsorb negatively charged bacterium, have good bactericidal effect, be widely used.But it is common
Quaternary ammonium salt chemical activity is lower, and when application exists substantially with free state, and toxicity is relatively large, and irritation is also strong, as anti-
Microbial inoculum application is dissolution type on the textile, is easily eluted, and be easily progressively enriched in human body surface, and long-time service is also easy to produce disease
Become.
Organosilicon quaternary ammonium salt is the ideal antibacterial agent of a kind of comprehensive performance, is generally used for the final finishing of fabric, is arranged
Fabric afterwards not only has excellent anti-microbial property, and is also equipped with good water suction absorption of perspiration, flexibility, flatness, rebound
Property, static electricity resistance and resistance tocrocking.The surfactant is non-stimulated to human skin and carcinogenesis, indices all meet state
The inside and outside requirement to antibacterial fabric.But the surface due to being attached to fabric after organosilicon quaternary ammonium salt again final finishing, pass through
After the washing of a period of time, gradually it is lost, it can not prolonged retention property.
It is modified in inorganic filler with organosilicon quaternary ammonium salt, modified inorganic filler can be made to have preferable
Biocidal property.(" West China dentistry is miscellaneous for document " synthesis of novel nano antibacterial inorganic filler and its Primary Study of anti-microbial property "
Will " in October, 2012, volume 30, the 5th phase, 526-530 pages) it reports N, N, N- trimethyl -3- (trimethoxy silicon substrate) third
Base -1- ammonium iodide is grafted to nanometer silicon dioxide particle surface, obtains quaternary ammonium salt modification nano silica, has stronger kill
Bacterium effect.But the polarity spectrum of quaternary ammonium salt and resin is larger, and quaternary ammonium salt modification nano silica is added to meeting in resin
There are problems that poor dispersion.
Tai Ji stone is natural rare mineral matter, has excellent far infrared function, and far infrared transmissivity reaches 91.7-
93.36%, far infrared acts on 3.9-16 μm of wavelength, and the far infrared wavelength beneficial to human body is 8-14 μm, and Tai Ji stone is not
Containing any radioactive substance being harmful to the human body, any harmful substance also forbidden without containing EU REACH Legislation, therefore too
Pole stone is highly beneficial to human body.Tai Ji stone raw ore is smashed and wears into micron-sized powder, then micron-sized powder nanosizing is made and is received
Meter level Tai Ji stone, is added in textile, not only advantageous to human health, and can be with antiultraviolet.
Currently, had on the market it is some addition nanometer Tai Ji works made of stones textiles, including underwear, underpants, socks,
Brassiere etc. has preferable far infrared transmission performance through research.Requirement with people to healthy living is higher and higher, to knitting
Object, the antibiotic property of especially personal fabric require higher and higher.But the bacteria resistance function of Tai Ji stone is relatively common, it can not be effective
Make textile fabrics that there is preferable bacteria resistance function, it usually needs some fungicide are added in textile.
Document " exploitation of antibacterial far infrared polypropylene fibre " (periodical " fabrics for industrial use " 2017, volume 35, the 7th
Phase, the 12-15 pages) report that the sodium zirconium phosphate with antibacterial functions is added in polypropylene fibre using co-blended spinning method is copper-loaded
Material and Tai Ji stone material with far-infrared functional, obtain a kind of novel antibacterial far infrared polypropylene fibre, and bacteriostasis rate reaches
To 98% or more, far infrared normal emittance reaches 85% or more, and human bloodstream amount and Hemodynamic environment amplification are all 32% or more.
But above fiber with transmitting far infrared and bacteria resistance function, it needs to add Tai Ji stone and fungicide respectively,
Have the shortcomings that at high cost, complicated for operation.If the Tai Ji stone with bacteria resistance function can be added directly in the fibre, without additional
Addition fungicide can be obtained by the fiber of transmitting far infrared and bacteria resistance function.But there is presently no such reports.
Summary of the invention
(1) the technical issues of solving used
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of preparation sides of antimicrobial form polypropylene fibre
Method, the antimicrobial form polypropylene fibre antibiotic property prepared is good, washability is good, has far infrared transmission.
(2) technical solution
In order to solve the above-mentioned technical problem, the present invention adopts the following technical scheme that,
A kind of preparation method of antimicrobial form polypropylene fibre, includes the following steps,
S1: the co-modified nanometer Tai Ji stone of dodecyl group and quaternary ammonium salt group is melted with PP GRANULES
It is granulated, obtains modified polypropylene agglomerate；
S2: the modified polypropylene agglomerate and PP GRANULES that step S1 is obtained carry out melt spinning, and it is poly- to obtain antimicrobial form
Tacryl.
Preferably, the dodecyl group and the co-modified nanometer Tai Ji stone of quaternary ammonium salt group step by the following method
It is prepared,
S3: being added dodecyl trialkoxy silane and 3- chloropropyl trialkoxy silane in a reservoir, under stiring,
The dilute hydrochloric acid of mass concentration 0.05% is added dropwise, drips, continues stirring 0.5 hour, is warming up to micro- reflux, is stirred to react 2 hours,
Low-boiling-point substance is evaporated off, obtains the silane moiety hydrolytic condensate of the group of chloropropyl containing 3- and dodecyl group；
S4: according to parts by weight, it is by 100 parts of nanometer Tai Ji stones, 200 parts of dehydrated alcohols and 0.5~1.5 part of mass concentration
0.05% dilute hydrochloric acid is added in container, and the silane moiety hydrolytic condensate in 10~30 parts of step S3 is added, rises under stirring
Temperature is reacted 2 hours, filtering removes filtrate, filters out solid washes of absolute alcohol 3 times, in vacuum drying oven to the micro- reflux of system
It is dry to constant weight, obtain dodecyl group and the co-modified nanometer Tai Ji stone of 3- chloropropyl group；
S5: according to parts by weight, by dodecyl group in 100 parts of step S4 and 3- chloropropyl group is co-modified receives
Rice Tai Ji stone, 150 parts of dimethyl sulfoxides and 10~30 parts of tertiary amine compound mixing, are warming up to 100~110 DEG C, reaction under stirring
30~50 hours, it is filtered to remove filtrate, the solid filtered out with drying after washes of absolute alcohol 3 times to perseverance in a vacuum drying oven
Weight obtains dodecyl group and the co-modified nanometer Tai Ji stone of quaternary ammonium salt group.
It is furthermore preferred that alkoxy described in step S3 is selected from one or more of methoxyl group, ethyoxyl and isopropoxy
Mixture.
It is furthermore preferred that the weight of dodecyl trialkoxy silane described in step S3 and 3- chloropropyl trialkoxy silane
Amount is than being 5:1~1:5.
It is further preferred that the weight ratio of the dodecyl trialkoxy silane and 3- chloropropyl trialkoxy silane
For 2:1~1:2.
It is furthermore preferred that the molal quantity of water and dodecyl trialkoxy silane and 3- chlorine in dilute hydrochloric acid described in step S3
The sum of molal quantity of propyl trialkoxy silane is than being 0.3~1:1.
It is further preferred that the molal quantity of water and dodecyl trialkoxy silane and 3- chloropropyl in the dilute hydrochloric acid
The sum of molal quantity of trialkoxy silane is than being 0.5~0.7:1.
It is furthermore preferred that tertiary amine compound described in step S5 is selected from N, N- dimethyl n octyl tertiary amine, N, N- dimethyl n
Dodecyl tertiary amine, N, N- dimethyl n tetradecyl tertiary amine, N, N- dimethyl n cetyl tertiary amine and N, N- dimethyl n ten
Eight alkyl tertiary amines, N methyldiethanol amine, triethanolamine and N, one or more of accelerine mixture.
Preferably, group containing dodecyl described in step S1 and the co-modified nanometer Tai Ji stone of quaternary ammonium salt group and poly-
The weight ratio of particulate propylene is 1:9~3:7.
Preferably, the weight ratio of modified polypropylene agglomerate described in step S2 and PP GRANULES is 1:5~8.
The antimicrobial form polypropylene that the preparation method of antimicrobial form polypropylene fibre is prepared in a kind of any of the above-described embodiment
Fiber.
The antimicrobial form polypropylene that the preparation method of antimicrobial form polypropylene fibre is prepared in a kind of any of the above-described embodiment
Application of the fiber in weaving.
Silane coupling agent is usually used in the surface treatment of inorganic filler, for improving the compatibility of inorganic filler and polymer.
According to " similar compatibility principle ", the compatibility of polar group and polar polymer is preferable, non-polar group and non-polar polymer
Compatibility it is preferable.Polypropylene belongs to non-polar polymer, and quaternary ammonium salt group belongs to polar group, and alkyl group belongs to nonpolarity
Group, therefore, the compatibility of polypropylene and alkyl group are preferable, and the compatibility of polypropylene and quaternary ammonium salt group is poor.The present invention
By dodecyl trialkoxy silane and 3- chloropropyl trialkoxy silane in insufficient amount of water hydrolytic condensation, had
The silane moiety hydrolytic condensate of alkoxy, dodecyl group and 3- chloropropyl group.In silane moiety hydrolytic condensate
Unreacted alkoxy can continue hydrolysis under aqueous environments and generate silicone hydroxyl, and silicone hydroxyl is reacted with Tai Ji stone, so that silane
Hydrolytic condensate is grafted to a nanometer surface for Tai Ji stone, obtains dodecyl group and the co-modified nanometer of 3- chloropropyl group
Tai Ji stone, 3- chloropropyl group therein can be reacted with tertiary amine compound, obtain quaternary ammonium salt group, therefore obtain positive ten
Dialkyl group group and the co-modified nanometer Tai Ji stone of quaternary ammonium salt group, quaternary ammonium salt group therein have preferable bacteriostasis property.
The co-modified nanometer Tai Ji stone of dodecyl group and quaternary ammonium salt group is added in polypropylene, dodecyl group can
With raising and polyacrylic compatibility, dispersibility of the nanometer Tai Ji stone in polypropylene is improved, quaternary ammonium salt can provide biocidal property
Can, so that obtained antimicrobial form polypropylene fibre is more than that 4% (mass fraction) all has preferably in the additive amount of nanometer Tai Ji stone
Mechanical property, and good antimicrobial effect, washability are good, also have far infrared transmission performance.
(3) beneficial effect
Compared to the prior art, the invention has the benefit that (1) only need to add modified Nano Tai Ji stone can so that
Polypropylene fibre has transmitting far infrared and antibacterial performance simultaneously；(2) modified nanometer Tai Ji stone is in polypropylene fibre
Dispersed preferable, additive amount reaches 4% (mass percent), does not influence substantially on the mechanical property of fiber；(3) modified
The washability of polypropylene fibre is good, after repeatedly washing, then has preferable bacteriostasis property and transmitting far infrared.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, by embodiment to the present invention carry out into
One step elaborates, but is not intended to limit the present invention.
If not specified, the number in embodiment below is all parts by weight.
Prepare silane moiety hydrolytic condensate
At room temperature, 100 parts of dodecyl trimethoxies are added in the container with thermometer, stirring rod and condenser pipe
The hydrochloric acid water that 2.4 parts of mass concentrations are 0.05% is added dropwise after mixing evenly in silane and 20 parts of r-chloropropyl trimethoxyl silanes
Solution continues stirring 0.5 hour, is warming up to the micro- back flow reaction of system 2 hours, 80 DEG C of removing low-boiling-point substances obtain viscosity after dripping off
(25 DEG C) the colorless and transparent silane moiety hydrolysates 1 for 69mPas.FT-IR analysis shows that, in 1010-1121cm-1Occur strong
Broad peak is the absorption peak of Si-O-Si, in 2887cm-1And 1198cm-1Appearance belongs to methoxyl group (Si-OCH3) absorption peak,
3280cm-1Occur belonging to the absorption peak of silicone hydroxyl, 1169cm-1Absorption peak be C-Cl absorption peak, in 2969cm-1It is existing
Weak spike and 2927cm-1The strong spike in the presence of in illustrates that there are methyl in product.
At room temperature, 100 parts of dodecyl trimethoxies are added in the container with thermometer, stirring rod and condenser pipe
The hydrochloric acid water that 5.3 parts of mass concentrations are 0.05% is added dropwise after mixing evenly in silane and 50 parts of r-chloropropyl trimethoxyl silanes
Solution continues stirring 0.5 hour, is warming up to the micro- back flow reaction of system 2 hours, 80 DEG C of removing low-boiling-point substances obtain viscosity after dripping off
(25 DEG C) the colorless and transparent silane moiety hydrolysates 2 for 85mPas.FT-IR analysis shows that, in 1008-1120cm-1Occur strong
Broad peak is the absorption peak of Si-O-Si, in 2887cm-1And 1198cm-1Appearance belongs to methoxyl group (Si-OCH3) absorption peak,
3280cm-1Occur belonging to the absorption peak of silicone hydroxyl, 1169cm-1Absorption peak be C-Cl absorption peak, in 2969cm-1It is existing
Weak spike and 2927cm-1The strong spike in the presence of in illustrates that there are methyl in product.
At room temperature, 50 parts of dodecyl triethoxies are added in the container with thermometer, stirring rod and condenser pipe
The hydrochloric acid that 5.4 parts of mass concentrations are 0.05% is added dropwise after mixing evenly in silane and 100 parts of chloropropyl triethoxysilanes
Aqueous solution continues stirring 0.5 hour, is warming up to the micro- back flow reaction of system 2 hours, 80 DEG C of removing low-boiling-point substances are glued after dripping off
(25 DEG C) of the degree colorless and transparent silane moiety hydrolysates 3 for 97mPas.FT-IR analysis shows that, in 1010-1121cm-1Occur
Strong broad peak is the absorption peak of Si-O-Si, in 2927cm-1Appearance belongs to Si-O-CH2CH3In-CH2Absorption peak, in 3280cm-1Occur belonging to the absorption peak of silicone hydroxyl, 1169cm-1Absorption peak be C-Cl absorption peak, in 2969cm-1Existing weak spike
And 2927cm-1The strong spike in the presence of in illustrates that there are methyl in product.
At room temperature, 20 parts of dodecyl triethoxies are added in the container with thermometer, stirring rod and condenser pipe
The hydrochloric acid that 8.5 parts of mass concentrations are 0.05% is added dropwise after mixing evenly in silane and 100 parts of chloropropyl triethoxysilanes
Aqueous solution continues stirring 0.5 hour, is warming up to the micro- back flow reaction of system 2 hours, 80 DEG C of removing low-boiling-point substances are glued after dripping off
(25 DEG C) of the degree colorless and transparent silane moiety hydrolysates 4 for 113mPas.
Prepare dodecyl group and the co-modified nanometer Tai Ji stone of 3- chloropropyl group
The dilute hydrochloric acid that 100 parts of nanometer Tai Ji stones, 200 parts of dehydrated alcohols and 0.5 part of mass concentration are 0.05% is added to
In container, 10 parts of silane moiety hydrolytic condensates 1 are added, the micro- reflux of system is warming up under stirring, react 2 hours, filter, remove
Filtrate filters out solid washes of absolute alcohol 3 times, dries in 60 DEG C of vacuum drying ovens to constant weight, obtains dodecyl group
The nanometer Tai Ji stone 1 co-modified with 3- chloropropyl group.FT-IR analysis shows that, in 1015-1128cm-1There is a strong peak in place,
For the absorption peak of Si-O-Si, in 1168cm-1Middle intensity spike, be C-Cl absorption peak, in 2967cm-1Existing weak point
Peak and 2926cm-1The strong spike in the presence of in illustrates that there are methyl in product.Product is used washes of absolute alcohol 3 times again, in 60 DEG C of vacuum
It dries in baking oven to constant weight, is then analyzed again with FT-IR, be shown in 1168cm-1There is the spike of same intensity in place, shows silane
Partial hydrolysis condensate 1 is by chemical bonds on Tai Ji stone surface.
The dilute hydrochloric acid that 100 parts of nanometer Tai Ji stones, 200 parts of dehydrated alcohols and 1 part of mass concentration are 0.05% is added to appearance
In device, 20 parts of silane moiety hydrolytic condensates 2 are added, the micro- reflux of system is warming up under stirring, react 2 hours, filtering removes filter
Liquid filters out solid washes of absolute alcohol 3 times, dries in 60 DEG C of vacuum drying ovens to constant weight, obtain dodecyl group and
The co-modified nanometer Tai Ji stone 2 of 3- chloropropyl group.FT-IR analysis shows that, in 1013-1127cm-1There is a strong broad peak in place,
For the absorption peak of Si-O-Si, in 1168cm-1Middle intensity spike, be C-Cl absorption peak, in 2967cm-1Existing weak point
Peak and 2926cm-1The strong spike in the presence of in illustrates that there are methyl in product.Product is cleaned 3 times with isopropanol again, is dried in 60 DEG C of vacuum
It dries in case to constant weight, then is analyzed with FT-IR, be shown in 1168cm-1There is the spike of same intensity in place, shows silane moiety water
Condensation product 2 is solved by chemical bonds on Tai Ji stone surface.
The dilute hydrochloric acid that 100 parts of nanometer Tai Ji stones, 200 parts of dehydrated alcohols and 1 part of mass concentration are 0.05% is added to appearance
In device, 20 parts of silane moiety hydrolytic condensates 3 are added, the micro- reflux of system is warming up under stirring, react 2 hours, filtering removes filter
Liquid filters out solid washes of absolute alcohol 3 times, dries in 60 DEG C of vacuum drying ovens to constant weight, obtain dodecyl group and
The co-modified nanometer Tai Ji stone 3 of 3- chloropropyl group.
The dilute hydrochloric acid that 100 parts of nanometer Tai Ji stones, 200 parts of dehydrated alcohols and 1 part of mass concentration are 0.05% is added to appearance
In device, 30 parts of silane moiety hydrolytic condensates 4 are added, the micro- reflux of system is warming up under stirring, react 2 hours, filtering removes filter
Liquid filters out solid washes of absolute alcohol 3 times, dries in 60 DEG C of vacuum drying ovens to constant weight, obtain dodecyl group and
The co-modified nanometer Tai Ji stone 4 of 3- chloropropyl group.
Prepare dodecyl group and the co-modified nanometer Tai Ji stone of quaternary ammonium salt group
By co-modified 1, the 150 part of dimethyl Asia of nanometer Tai Ji stone of 100 parts of dodecyl groups and 3- chloropropyl group
Sulfone and 10 parts of N, the mixing of N- dimethyl n octadecyl tertiary amine, are warming up to 100 DEG C under stirring, react 50 hours, be filtered to remove filter
Liquid, the solid filtered out with drying in a vacuum drying oven to constant weight after washes of absolute alcohol 3 times, obtain dodecyl group and
The co-modified nanometer Tai Ji stone 1 of quaternary ammonium salt group.FT-IR analysis shows that, 1015-1129cm-1There is a Qiang Kuanfeng at place, is Si-O-
The characteristic absorption peak of Si, 958cm-1The peak of the moderate strength at place is the characteristic absorption peak of quaternary ammonium salt.It is instruction with bromophenol blue-ethyl alcohol
Agent show that the quaternary ammonium rate of product is 76.3% using hydrochloric acid-ethyl alcohol titration.
By co-modified 2, the 150 parts of dimethyl Asias of nanometer Tai Ji stone of 100 parts of dodecyl groups and 3- chloropropyl group
Sulfone and 20 parts of N, the mixing of N- dimethyl n octyl tertiary amine, are warming up to 100 DEG C under stirring, react 50 hours, be filtered to remove filtrate, filter
Solid out obtains dodecyl group and quaternary ammonium with drying in a vacuum drying oven to constant weight after washes of absolute alcohol 3 times
The co-modified nanometer Tai Ji stone 2 of salt groups.FT-IR analysis shows that, 1013-1128cm-1There is a Qiang Kuanfeng at place, is Si-O-Si's
Characteristic absorption peak, 958cm-1The peak of the moderate strength at place is the characteristic absorption peak of quaternary ammonium salt.Using bromophenol blue-ethyl alcohol as indicator,
The quaternary ammonium rate that product is obtained using hydrochloric acid-ethyl alcohol titration is 78.1%.
By co-modified 3, the 150 parts of dimethyl Asias of nanometer Tai Ji stone of 100 parts of dodecyl groups and 3- chloropropyl group
Sulfone and 20 parts of N- ethyldiethanolamine mixing, are warming up to 110 DEG C, react 30 hours, be filtered to remove filtrate, what is filtered out consolidates under stirring
Body obtains dodecyl group and quaternary ammonium salt group with drying in a vacuum drying oven to constant weight after washes of absolute alcohol 3 times
Co-modified nanometer Tai Ji stone 3.Using bromophenol blue-ethyl alcohol as indicator, the quaternized of product is obtained using hydrochloric acid-ethyl alcohol titration
Rate is 72.5%.
By co-modified 4, the 150 parts of dimethyl Asias of nanometer Tai Ji stone of 100 parts of dodecyl groups and 3- chloropropyl group
Sulfone and 30 parts of N, the mixing of N- dimethyl n dodecyl tertiary amine, are warming up to 100 DEG C under stirring, react 40 hours, be filtered to remove filter
Liquid, the solid filtered out with drying in a vacuum drying oven to constant weight after washes of absolute alcohol 3 times, obtain dodecyl group and
The co-modified nanometer Tai Ji stone 4 of quaternary ammonium salt group.Using bromophenol blue-ethyl alcohol as indicator, must be produced using hydrochloric acid-ethyl alcohol titration
The quaternary ammonium rate of object is 77.9%.
Embodiment 1
By the co-modified nanometer Tai Ji stone 1 of 10 parts of dodecyl groups and quaternary ammonium salt group and 90 parts of PP GRANULESs into
Row melt pelletization obtains modified polypropylene agglomerate 1；
10 parts of modified polypropylene agglomerate 1 and 70 part PP GRANULESs are subjected to melt spinning, it is fine to obtain antimicrobial form polypropylene
Dimension 1.Melt-spinning technology: 250 DEG C of spinning temperature, draw ratio 3.5, spinning speed 800m/min.
Embodiment 2
By the co-modified nanometer Tai Ji stone 2 of 20 parts of dodecyl groups and quaternary ammonium salt group and 80 parts of PP GRANULESs into
Row melt pelletization obtains modified polypropylene agglomerate 2；
10 parts of modified polypropylene agglomerate 2 and 70 part PP GRANULESs are subjected to melt spinning, it is fine to obtain antimicrobial form polypropylene
Dimension 2.Melt-spinning technology is consistent with embodiment 1.
Embodiment 3
By the co-modified nanometer Tai Ji stone 3 of 30 parts of dodecyl groups and quaternary ammonium salt group and 70 parts of PP GRANULESs into
Row melt pelletization obtains modified polypropylene agglomerate 3；
10 parts of modified polypropylene agglomerate 3 and 60 part PP GRANULESs are subjected to melt spinning, it is fine to obtain antimicrobial form polypropylene
Dimension 3.Melt-spinning technology is consistent with embodiment 1.
Embodiment 4
By the co-modified nanometer Tai Ji stone 4 of 30 parts of dodecyl groups and quaternary ammonium salt group and 70 parts of PP GRANULESs into
Row melt pelletization obtains modified polypropylene agglomerate 4；
10 parts of modified polypropylene agglomerate 4 and 50 part PP GRANULESs are subjected to melt spinning, it is fine to obtain antimicrobial form polypropylene
Dimension 4.Melt-spinning technology is consistent with embodiment 1.
Embodiment 5
By the co-modified nanometer Tai Ji stone 2 of 15 parts of dodecyl groups and quaternary ammonium salt group and 85 parts of PP GRANULESs into
Row melt pelletization obtains modified polypropylene agglomerate 5；
10 parts of modified polypropylene agglomerate 5 and 80 part PP GRANULESs are subjected to melt spinning, it is fine to obtain antimicrobial form polypropylene
Dimension 5.Melt-spinning technology is consistent with embodiment 1.
Embodiment 6
By the co-modified nanometer Tai Ji stone 3 of 20 parts of dodecyl groups and quaternary ammonium salt group and 80 parts of PP GRANULESs into
Row melt pelletization obtains modified polypropylene agglomerate 6；
10 parts of modified polypropylene agglomerate 6 and 70 part PP GRANULESs are subjected to melt spinning, it is fine to obtain antimicrobial form polypropylene
Dimension 6.Melt-spinning technology is consistent with embodiment 1.
Embodiment 7
By the co-modified nanometer Tai Ji stone 3 of 10 parts of dodecyl groups and quaternary ammonium salt group and 90 parts of PP GRANULESs into
Row melt pelletization obtains modified polypropylene agglomerate 7；
10 parts of modified polypropylene agglomerate 7 and 60 part PP GRANULESs are subjected to melt spinning, it is fine to obtain antimicrobial form polypropylene
Dimension 7.Melt-spinning technology is consistent with embodiment 1.
Comparative example 1
10 parts of unmodified nanometer Tai Ji stones and 90 parts of PP GRANULESs are subjected to melt pelletization, obtain modified polypropylene agglomerate
8；
10 parts of modified polypropylene agglomerate 8 and 80 part PP GRANULESs are subjected to melt spinning, obtain modified polypropylene fiber
8.Melt-spinning technology is consistent with embodiment 1.
Comparative example 2
20 parts of unmodified nanometer Tai Ji stones and 80 parts of PP GRANULESs are subjected to melt pelletization, obtain modified polypropylene agglomerate
9；
10 parts of modified polypropylene agglomerate 9 and 60 part PP GRANULESs are subjected to melt spinning, obtain modified polypropylene fiber
9.Melt-spinning technology is consistent with embodiment 1.
Performance test
Far infrared transmissivity: it refers to GB/T30127-2013 " detection and evaluation of textile far infrared performance ", at 34 DEG C
It is tested using the DR915G textile far infrared transmissivity tester of Wenzhou Darong Textile Instrument Co., Ltd.'s production to test sample
Normal direction far infrared transmissivity of the product at 5~14 μm.Concrete outcome is as shown in table 1.
Mechanical property: referring to GB/T14344-2008 " chemical fiber filament Erichsen test method ", uses at 25 DEG C
YG (B) 021H type chemical-fibres filaments electronics strength machine test sample to be tested of Wenzhou Darong Textile Instrument Co., Ltd.'s production breaks
Resistance to spalling, elongation at break and initial modulus.Concrete outcome is as shown in table 1.
Biocidal property: it refers to GB/T20944.3-2008 " the evaluation third portion of antibacterial textile performance: succusion ", strain
Select staphylococcus aureus and Escherichia coli.Concrete outcome is as shown in table 1.
1 sample to be tested the performance test results of table
From the results shown in Table 1, antimicrobial form polypropylene fibre biocidal property of the invention is relatively good, and has preferable
Far infrared transmission performance, and with the increasing of dodecyl group and the co-modified nanometer Tai Ji stone content of quaternary ammonium salt group
Add, antimicrobial form polypropylene fibre has better biocidal property, while co-modified in dodecyl group and quaternary ammonium salt group
When nanometer Tai Ji stone additive amount is no more than 4% (mass fraction), antimicrobial form polypropylene fibre has better mechanical property.
Washability test: by the antimicrobial form polypropylene fibre of embodiment 1-9 after 50 standard wash, according to above-mentioned remote
Infrared emittance and the test of the test method of biocidal property.Concrete outcome is as shown in table 2.
2 sample to be tested the performance test results of table
| Example | Far infrared transmissivity/% | Biocidal property/% |
| Embodiment 1 | 80.8 | 60.3 |
| Embodiment 2 | 83.5 | 77.5 |
| Embodiment 3 | 87.4 | 92.1 |
| Embodiment 4 | 88.9 | 97.6 |
| Embodiment 5 | 81.8 | 74.8 |
| Embodiment 6 | 82.3 | 88.7 |
| Embodiment 7 | 80.9 | 85.4 |
| Comparative example 1 | 81.6 | 12.4 |
| Comparative example 2 | 83.7 | 17.3 |
From the results shown in Table 2, antimicrobial form polypropylene fibre of the invention has preferable washability.
In conclusion antimicrobial form polypropylene fibre of the invention has preferable biocidal property, far infrared transmission performance, Er Qieli
Better performances are learned, washability is preferable.
It should be noted that embodiment disclosed above only embodies and illustrates technical solution of the present invention, rather than it is used to limit this
The protection scope of invention, although explaining in detail referring to preferred embodiment to the present invention, any those skilled in the art is answered
Work as understanding, modify within the scope of technical solution of the present invention or various change, equivalent replacement not departing from, this all should belong to
The protection scope of invention.
Claims (10)
1. a kind of preparation method of antimicrobial form polypropylene fibre, it is characterised in that: include the following steps,
S1: the co-modified nanometer Tai Ji stone of dodecyl group and quaternary ammonium salt group is subjected to melting with PP GRANULES and is made
Grain, obtains modified polypropylene agglomerate；
S2: the modified polypropylene agglomerate and PP GRANULES that step S1 is obtained carry out melt spinning, obtain antimicrobial form polypropylene
Fiber.
2. the preparation method of antimicrobial form polypropylene fibre according to claim 1, it is characterised in that: the dodecyl
By the following method prepared by step for group and the co-modified nanometer Tai Ji stone of quaternary ammonium salt group,
S3: being added dodecyl trialkoxy silane and 3- chloropropyl trialkoxy silane in a reservoir, under stiring, is added dropwise
The dilute hydrochloric acid of mass concentration 0.05%, drips, and continues stirring 0.5 hour, is warming up to micro- reflux, is stirred to react 2 hours, is evaporated off
Low-boiling-point substance obtains the silane moiety hydrolytic condensate of the group of chloropropyl containing 3- and dodecyl group；
S4: according to parts by weight, it is by 100 parts of nanometer Tai Ji stones, 200 parts of dehydrated alcohols and 0.5~1.5 part of mass concentration
0.05% dilute hydrochloric acid is added in container, and the silane moiety hydrolytic condensate in 10~30 parts of step S3 is added, rises under stirring
Temperature is reacted 2 hours, filtering removes filtrate, filters out solid washes of absolute alcohol 3 times, in vacuum drying oven to the micro- reflux of system
It is dry to constant weight, obtain dodecyl group and the co-modified nanometer Tai Ji stone of 3- chloropropyl group；
S5: according to parts by weight, too by the co-modified nanometer of dodecyl group in 100 parts of step S4 and 3- chloropropyl group
Pole stone, 150 parts of dimethyl sulfoxides and the mixing of 10~30 parts of tertiary amine compounds, are warming up to 100~110 DEG C under stirring, and reaction 30~
50 hours, it is filtered to remove filtrate, the solid filtered out is obtained with drying in a vacuum drying oven to constant weight after washes of absolute alcohol 3 times
The nanometer Tai Ji stone co-modified to dodecyl group and quaternary ammonium salt group.
3. the preparation method of antimicrobial form polypropylene fibre according to claim 2, it is characterised in that: alkane described in step S3
Oxygroup is selected from one or more of methoxyl group, ethyoxyl and isopropoxy mixture.
4. the preparation method of antimicrobial form polypropylene fibre according to claim 2, it is characterised in that: described in step S3 just
The weight ratio of dodecyl trialkoxy silane and 3- chloropropyl trialkoxy silane is 5:1~1:5.
5. the preparation method of antimicrobial form polypropylene fibre according to claim 2, it is characterised in that: dilute described in step S3
The sum of molal quantity of the molal quantity of water and dodecyl trialkoxy silane and 3- chloropropyl trialkoxy silane ratio in hydrochloric acid
For 0.3~1:1.
6. the preparation method of antimicrobial form polypropylene fibre according to claim 2, it is characterised in that: uncle described in step S5
Amine compounds are selected from N, N- dimethyl n octyl tertiary amine, N, N- dimethyl n dodecyl tertiary amine, N, N- dimethyl n tetradecyl
Tertiary amine, N, N- dimethyl n cetyl tertiary amine and N, N- dimethyl n octadecyl tertiary amine, N methyldiethanol amine, three ethyl alcohol
Amine and N, one or more of accelerine mixture.
7. the preparation method of antimicrobial form polypropylene fibre according to claim 1, it is characterised in that: contain described in step S1
The weight ratio of dodecyl group and the co-modified nanometer Tai Ji stone and PP GRANULES of quaternary ammonium salt group is 1:9~3:7.
8. the preparation method of antimicrobial form polypropylene fibre according to claim 1, it is characterised in that: change described in step S2
Property polypropylene agglomerate and PP GRANULES weight ratio be 1:5~8.
9. a kind of antimicrobial form poly- third that the preparation method of the described in any item antimicrobial form polypropylene fibres of claim 1-8 is prepared
Alkene fiber.
10. a kind of antimicrobial form that the preparation method of the described in any item antimicrobial form polypropylene fibres of claim 1-8 is prepared
Application of the polypropylene fibre in weaving.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111593432A (en) * | 2020-05-26 | 2020-08-28 | 苏州金莱特化纤有限公司 | Anti-corrosion and anti-bacterial functional fiber and preparation process thereof |
| CN112759662A (en) * | 2021-01-18 | 2021-05-07 | 福建农林大学 | Separation and purification method of tremella polysaccharide |
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| CN103535372A (en) * | 2013-10-09 | 2014-01-29 | 江苏惠兴康科技有限公司 | Curable composite quaternary ammonium salt, preparation method thereof, and application thereof in disinfection and sterilization |
| CN107694522A (en) * | 2017-10-16 | 2018-02-16 | 广州中国科学院工业技术研究院 | Nano-particle containing organosilicon quaternary ammonium salt and its production and use |
| CN109320999A (en) * | 2018-11-26 | 2019-02-12 | 福建省银河服饰有限公司 | A kind of quaternized nanometer Tai Ji stone and preparation method thereof and modified polypropylene fiber |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103535372A (en) * | 2013-10-09 | 2014-01-29 | 江苏惠兴康科技有限公司 | Curable composite quaternary ammonium salt, preparation method thereof, and application thereof in disinfection and sterilization |
| CN107694522A (en) * | 2017-10-16 | 2018-02-16 | 广州中国科学院工业技术研究院 | Nano-particle containing organosilicon quaternary ammonium salt and its production and use |
| CN109320999A (en) * | 2018-11-26 | 2019-02-12 | 福建省银河服饰有限公司 | A kind of quaternized nanometer Tai Ji stone and preparation method thereof and modified polypropylene fiber |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111593432A (en) * | 2020-05-26 | 2020-08-28 | 苏州金莱特化纤有限公司 | Anti-corrosion and anti-bacterial functional fiber and preparation process thereof |
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| CN112759662A (en) * | 2021-01-18 | 2021-05-07 | 福建农林大学 | Separation and purification method of tremella polysaccharide |
| CN112759662B (en) * | 2021-01-18 | 2021-12-28 | 福建农林大学 | Separation and purification method of tremella polysaccharide |
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