CN100457988C - Antibacterial PET fiber and process for making same - Google Patents
Antibacterial PET fiber and process for making same Download PDFInfo
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- CN100457988C CN100457988C CNB2006100231618A CN200610023161A CN100457988C CN 100457988 C CN100457988 C CN 100457988C CN B2006100231618 A CNB2006100231618 A CN B2006100231618A CN 200610023161 A CN200610023161 A CN 200610023161A CN 100457988 C CN100457988 C CN 100457988C
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Abstract
The invention provides an antibiotic PET fiber with silver nanometer zinc oxide, relative preparation method and application. The invention uses the method of composite spinning to add the silver nanometer zinc oxide into the layer of terylene, while prepared modified terylene has higher antibiotic sterilize ability. The invention can apply the mass continuous production of fusion spinning modified terylene.
Description
Technical field
The invention belongs to and relate to a kind of antibacterial PET fiber and preparation method thereof, relate in particular to a kind of antibacterial PET fiber by the silver-carrying zinc oxide nano-particle modification and preparation method thereof.
Background technology
In actual life, people unavoidably can touch microorganisms such as various bacteriums, fungi.These microorganisms are the ramp breeding under suitable environmental condition, and spreads disease by contact, influences the healthy of people.In the daily life, all kinds of textiless are the ground of the good existence of these microorganisms, also are the important propagating sources of disease, and the human lives is among the encirclement of microorganism.Fiber can absorb a lot of microorganisms, if temperature is suitable, these microorganisms will breed rapidly, and human body is produced all harm.In recent years, the antibiotic property of fibre more and more is subjected to people's attention.Have the fiber of antibacterial action and the research of textiles extremely important meaning is arranged.The function and the use value of anti-bacterial fibre comprise the following aspects:
1. many bacterioneustons of hospital environment all have the very big possibility of carrying disease germs on the clothes of doctor and patient and the hospital textiles commonly used, not only are easy to cause the cross infection between the patient, also can bring healthy people germ or in the environment of disease propagation beyond the hospital.It is no doubt important to sterilize, but can only intermittently carry out.To the staphylococcus aureus that pathogenicity easily develops immunity to drugs again by force, use antibiotic fabric to be suppressed, more necessary.
2. antibiotic is the important measures of strengthening food hygiene
In the per pass operation of food processing, all to prevent the Food Contact bacterium.As food processing factory, provisions shop, dining room, restaurant and even family kitchen, an importance of dust alleviation work, Work Clothes, apron, rag, food drape etc. must have antibiotic and harmless function.
3. antibiotic is the effective way of Creating Comfort living environment
Bacterium on the daily textiles is breeding rapidly in living environment, and its sanitary condition is worsened, and particularly the temperature in clothes, bed clothes and the ornament often creates good conditions for the breeding of growing of bacterium.These bacteriums have golden yellow staphylococcus, Escherichia coli, black-koji mould etc., even some bacterium is the non-pathogenic bacteria class, also can produce certain pathology stimulates, especially when clothes and bed clothes stain sweat that human secretory is arranged and sebum, because the decomposition of bacterium, can produce foreign odors such as ammonia, it is worried that these body odors increase often for life.For this reason, need use modern means of science and technology to prepare high-grade antibiotic fabric, pursue comfortable and needs healthy living to be fit to people.
4. antibiotic also is protection to the fiber itself performance
Textiles owing to the influence of dirt on high-temperature high humidity climate and the clothing, also can constitute the strong condition of mold propagates between resting period, not only make painted, the variable color of dress material, and make the dress material embrittlement rotten, even go back entail dangers to skin when wearing.In order to prevent the generation of this class situation, antibacterial and mouldproof also should be the necessary additional function of grade textiles.
The key issue of improving the anti-microbial property of chemical fibre is how when improving the anti-microbial property of fiber, also keeps the original excellent mechanical property of fiber.For making fiber reach desirable antibacterial effect, produce anti-bacterial fibre, current, anti-bacterial fibre is presenting diversified development circumstances, and its variation not only is the different of fiber base material and antiseptic, and is the technological approaches difference of anti-bacterial fibre exploitation.Make the chemical fibre modification or make it to obtain some function by additive, absorb or performance such as photocatalysis is one of important method of preparation modifying chemical fiber as antibiotic and sterilizing, antistatic, uvioresistant.Conclude its state of the art, can be divided into four aspects:
1. the employing chemical technology is grafted to antibiotic group on the reactive group of fiber surface.For the material that does not possess reactive group, introduce reactive group, make fiber possess the condition of chemical modification.
2. adopt the physical modification technology, make antiseptic infiltrated fiber top layer than the position, deep.Such as, develop the fiber of shaggy microporeization, when the arrangement of back, help below the antiseptic infiltrated fiber top layer; Can also be spiked into antiseptic within the spinning oil in spinning process, antiseptic can be included in the position below the top layer when the condensation contraction of fiber and drawing-off are shunk.
3. in carrying out wet spinning, in spinning bath, add antiseptic, also can receive good antibacterial effect.
4. antiseptic is mixed and spun fiber in the spinning solution, this is the main means of exploitation anti-bacterial fibre.Generally say, adopt inorganic antiseptic to adopt melt spinning method more, adopt organic antibacterial agent to adopt solution spinning more.
But at present exist antiseptic bad dispersibility in fiber in the blending technology, the antiseptic consumption is big, and utilization rate is low, and problem such as waste raw material.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of antibacterial PET fiber and preparation method thereof, with the shortcoming of aspects such as solving antibacterial effect in the prior art and security is relatively poor, waste antiseptic raw material, cost of investment are big.
Principle of the present invention is: in order to solve the dispersion problem of antiseptic in fiber, reach antiseptic and the good compatibility of PET matrix, the present invention has at first studied the technology of the silver-carrying zinc oxide nano-particle particle being carried out finishing; Again by selecting the dispersant of favorable dispersibility, made the antibacterial PET master batch of high concentration, adopted the compound spining technology that spins of core-skin fusion at last, antiseptic has been doped in the cortex, this not only saves the antiseptic raw material, and helps keeping the key property of fiber.
The present invention at first provides a kind of antibacterial PET fiber, contains the silver-carrying zinc oxide nano-particle that percentage by weight is 1-5% in this antibacterial PET fiber.
The present invention also provides the preparation method of this antibacterial PET fiber, and this method comprises the following steps:
(1) preparation silver-carrying zinc oxide nano-particle and modifying: in the process of preparation nano zine oxide with metal A g
+Be doped in the middle of the zinc oxide, obtain silver-carrying zinc oxide nano-particle; Adding weight ratio in container is 10-100: 1 silver-carrying zinc oxide nano-particle and silane coupler (KH-560) are solvent with the absolute ethyl alcohol, 78 ℃～80 ℃ stirring and refluxing 2-4 hour; With the sample oven dry porphyrize of handling well;
(2) preparation antibacterial PET master batch (being granulation): silver-carrying zinc oxide nano-particle, dispersant and the pure PET of modified are cut into slices according to 15-25: 1: the mass ratio of 30-50 is extruded by the double screw extruder blend, carry out pelletizing by pelleter then, make the antibacterial PET master batch; Wherein granulation process is respectively distinguished temperature range and is followed successively by: 165 ℃～200 ℃, 265 ℃～285 ℃, 265 ℃～285 ℃, 265～285 ℃, 260～285 ℃; Wherein dispersant is for adopting conventional dispersant, as Tissuemat E 1# or 2#, BH-2 etc.
(3) spinning has skin--the antibacterial PET fiber of cored structure: be that 20%～30% antibacterial PET master batch is to join in the cortex with respect to 2%～6% of total weight of fiber with antiseptic content, pure PET is as sandwich layer, Pi Yuxin is according to 1: the part by weight of 4-5 adds respectively in the double screw extruder, spins out to have skin--the antibacterial PET fiber of cored structure; Wherein spinning technology parameter is:
Sandwich layer: each is distinguished temperature and is respectively 280 ℃～290 ℃, and 280 ℃～300 ℃, 280 ℃～300 ℃, 280 ℃～300 ℃; The measuring pump temperature is 280 ℃～297 ℃, and return bend temperature is 280 ℃～297 ℃; Screw speed is 41～55rpm; Pressure is 41～60 kilograms; For pump amount 5～8g/min;
Cortex: each is distinguished temperature and is respectively 280 ℃～290 ℃, and 280 ℃～300 ℃, 280 ℃～300 ℃, 280 ℃～300 ℃; The measuring pump temperature is 280 ℃～297 ℃, and return bend temperature is 280 ℃～297 ℃, and spin manifold temperature is 290 ℃～310 ℃; Screw speed is 40～50rpm, and pressure is 30～40 kilograms; For pump amount 20～25g/min;
The technological parameter of drawtwister: draft temperature, temperature of heat plate are about 80 ℃, and hot plate temperature is about 160 ℃, and draw speed is 801～900m/min; Draw ratio: 4～5 times.
This antibacterial PET fiber can be used for preparing antibiotic clothing or fabric.
The modified dacron of being made up of pure PET terylene chips, silver-carrying zinc oxide nano-particle, dispersant etc. provided by the invention has higher mechanical property and good antibiotic and sterilizing effect, and can implement industrial batch production.The antibiotic polyester fiber that is spun is carried out the antibacterial effect test, and with reference to FZ/T 01021-92 (antibacterial fabric method for testing performance), the anti-biotic material (goods) that GB 15979-2002. and japanese food analysis center the formulate method of dripping is carried out.The antibacterial PET fiber that records 1% antiseptic content can reach more than 99% the killing rate of Escherichia coli and staphylococcus aureus.
The specific embodiment
The invention will be further described below in conjunction with example.
Example 1:
Adding 10 gram silver-carrying zinc oxide nano-particle powders in three-neck flask, 0.3 gram silane coupler (KH-560) is added wherein, was solvent with the absolute ethyl alcohol, 78 ℃ of stirring and refluxing 2.5 hours.With the sample oven dry porphyrize of handling well, obtain the silver-carrying zinc oxide nano-particle particle of finishing.
Example 2:
Adding 30 gram silver-carrying zinc oxide nano-particle powders in three-neck flask, 1 gram silane coupler (KH-560) is added wherein, was solvent with the absolute ethyl alcohol, 80 ℃ of stirring and refluxing 3 hours.With the sample oven dry porphyrize of handling well, obtain the silver-carrying zinc oxide nano-particle particle of finishing.
Example 3:
With quality is year silver (Ag that silane coupler KH-560 (modifying dosage is 2%) carries out finishing that passes through of 300 grams
+Content is 3%) (dry pure PET section blend on double screw extruder is extruded after Tissuemat E-1#) and the pre-crystallization of 680 grams, and granulation process is respectively distinguished temperature and is followed successively by 165 ℃, 265 ℃, 265 ℃, 265 ℃, 260 ℃ for nanometer Zinc oxide powder, 20 gram dispersants.Then by the plastic grain cutting machine pelletizing.Obtain having the good antibacterial matrices of dispersion effect of higher antiseptic content.
Example 4:
With quality is year silver (Ag that silane coupler KH-560 (the modification amount is 3%) carries out finishing that passes through of 100 grams
+Content is 3%) (dry pure PET section blend on double screw extruder is extruded after Tissuemat E-2#) and the pre-crystallization of 220 grams, and granulation process is respectively distinguished temperature and is followed successively by 200 ℃, 285 ℃, 285 ℃, 285 ℃, 285 ℃ for nanometer Zinc oxide powder, 5 gram dispersants.By the plastic grain cutting machine pelletizing, obtain having the good antibacterial matrices of dispersion effect of higher antiseptic content then.
Example 5:
With quality is year silver (Ag that coupling agent KH-560 (the modification amount is 3%) carries out finishing that passes through of 300 grams
+Content is 3%) the dry pure PET section blend on double screw extruder of nano zinc oxide particles, 20 gram dispersants (BH-2) and 680 grams extrudes, and granulation process is respectively distinguished temperature and is followed successively by 185 ℃, 275 ℃, 275 ℃, 275 ℃, 270 ℃.By the plastic grain cutting machine pelletizing, obtain having the good antibacterial matrices of dispersion effect of higher antiseptic content then.Adopt the method for common spinning, antibacterial dacron master batch and pure polyester slice are joined double screw extruder with 2: 8 ratio, spin out polyster fibre with antibacterial functions.Spinning technology parameter is: each is distinguished temperature and is respectively 285 ℃, and 297 ℃, 298 ℃, 298 ℃, the measuring pump temperature is 297 ℃, and return bend temperature is 297 ℃, and spin manifold temperature is 310 ℃.Screw speed 40rpm.For the pump amount is 34g/min.Head pressure remains unchanged in the spinning process, and spinning is smooth, does not have lousiness behind 4 times of the strand drawns.
Example 6:
With quality is year silver (Ag that silane coupler KH-560 (the modification amount is 3%) carries out finishing that passes through of 100 grams
+Content is 3%) (dry pure PET section blend on double screw extruder is extruded after Tissuemat E-2#) and the pre-crystallization of 226.7 grams, and granulation process is respectively distinguished temperature and is followed successively by 185 ℃, 275 ℃, 275 ℃, 275 ℃, 270 ℃ for nanometer Zinc oxide powder, 5 gram dispersants.By the plastic grain cutting machine pelletizing, obtain having the good antibacterial matrices of dispersion effect of higher antiseptic content then.
Adopt the method for skin-core composite spinning, the antibacterial PET master batch of certain mass is joined cortex, pure polyester slice is as sandwich layer, and skin and core gross mass add respectively in the double screw extruder with 2: 8 ratio, spin out to have skin--the antibacterial PET fiber of cored structure.Spinning technology parameter is:
Sandwich layer (pure PET): each is distinguished temperature and is respectively 280 ℃, and 280 ℃, 280 ℃, 280 ℃.The measuring pump temperature is 280 ℃, and return bend temperature is 280 ℃.Screw speed is 41rpm.Pressure is 41 kilograms.For pump amount 5g/min.
Cortex: each is distinguished temperature and is respectively 280 ℃, and 280 ℃, 280 ℃, 280 ℃.The measuring pump temperature is 280 ℃, and return bend temperature is 280 ℃, and spin manifold temperature is 290 ℃.Screw speed is 40rpm, and pressure is 30 kilograms.For pump amount 20g/min.Head pressure remains unchanged in the composite spinning process, and spinning is smooth, does not have lousiness behind 4 times of the strand drawns.The technological parameter of drawtwister:
Draft temperature: temperature of heat plate is 80 ℃, and hot plate temperature is 160 ℃, and draw speed is 801m/min.
Draw ratio: 4 times.
Example 7:
With quality is year silver (Ag that silane coupler KH-560 (the modification amount is 3%) carries out finishing that passes through of 200 grams
+Content is 3%) (dry pure PET section blend on double screw extruder is extruded after Tissuemat E-2#) and the pre-crystallization of 453.4 grams, and granulation process is respectively distinguished temperature and is followed successively by 195 ℃, 278 ℃, 278 ℃, 278 ℃, 270 ℃ for nanometer Zinc oxide powder, 10 gram dispersants.By the plastic grain cutting machine pelletizing, obtain having the good antibacterial matrices of dispersion effect of higher antiseptic content then.
Adopt the method for skin-core composite spinning, the antibacterial PET master batch of certain mass is joined cortex, pure polyester slice is as sandwich layer, and skin and core gross mass add respectively in the double screw extruder with 2: 8 ratio, spin out to have skin--the antibacterial PET fiber of cored structure.Spinning technology parameter is:
Sandwich layer (pure PET): each is distinguished temperature and is respectively 290 ℃, and 300 ℃, 300 ℃, 300 ℃.The measuring pump temperature is 297 ℃, and return bend temperature is 297 ℃.Screw speed is 55rpm.Pressure is 60 kilograms.For pump amount 8g/min.
Cortex: each is distinguished temperature and is respectively 290 ℃, and 300 ℃, 300 ℃, 300 ℃.The measuring pump temperature is 297 ℃, and return bend temperature is 297 ℃, and spin manifold temperature is 310 ℃.Screw speed is 50rpm, and pressure is 40 kilograms.For pump amount 25g/min.Head pressure remains unchanged in the composite spinning process, and spinning is smooth, does not have lousiness behind 4 times of the strand drawns.The technological parameter of drawtwister:
Draft temperature: temperature of heat plate is 80 ℃, and hot plate temperature is 160 ℃, and draw speed is 801m/min.
Draw ratio: 5 times.
Experimental program according to example 6, the antibiotic polyester fiber that is spun is carried out the antibacterial effect test, with reference to FZ/T 01021-92 (antibacterial fabric method for testing performance), the anti-biotic material (goods) that GB 15979-2002. and japanese food analysis center the formulate method of dripping is carried out.The compound PET of the spinning fiber that records 1% antiseptic content can reach more than 99% the killing rate of Escherichia coli and staphylococcus aureus.
Illustrate clearly that from above-mentioned example silver-carrying zinc oxide nano-particle modified dacron anti-bacterial fibre of the present invention has reached desirable antibacterial effect.
Claims (2)
1. antibacterial PET fiber is characterized in that containing in this antibacterial PET fiber percentage by weight and is 1%～5% silver-carrying zinc oxide nano-particle; Wherein silver-carrying zinc oxide nano-particle prepares by the following method: the preparation nano zine oxide process in metal A g
+Be doped in the middle of the zinc oxide, obtain silver-carrying zinc oxide nano-particle; Adding weight ratio in container is 10-100: 1 silver-carrying zinc oxide nano-particle and silane coupler are solvent with the absolute ethyl alcohol, 78 ℃～80 ℃ stirring and refluxing 2-4 hour; With the sample oven dry porphyrize of handling well.
2. a method for preparing the described antibacterial PET fiber of claim 1 is characterized in that this method comprises the following steps:
(1) preparation silver-carrying zinc oxide nano-particle and modifying: in the process of preparation nano zine oxide with metal A g
+Be doped in the middle of the zinc oxide, obtain silver-carrying zinc oxide nano-particle; Adding weight ratio in container is 10-100: 1 silver-carrying zinc oxide nano-particle and silane coupler are solvent with the absolute ethyl alcohol, 78 ℃～80 ℃ stirring and refluxing 2-4 hour; With the sample oven dry porphyrize of handling well;
(2) manufacturing of antibacterial PET master batch: silver-carrying zinc oxide nano-particle, dispersant and the pure PET of modified are cut into slices according to 15-25: 1: the mass ratio of 30-50 is extruded by the double screw extruder blend, carries out pelletizing by pelleter then, produces the antibacterial PET master batch; Wherein granulation process is respectively distinguished temperature range and is followed successively by: 165 ℃～200 ℃, 265 ℃～285 ℃, 265 ℃～285 ℃, 265 ℃～285 ℃, 260 ℃～285 ℃;
(3) spinning has the antibacterial PET fiber of skin-cored structure: be that 20%～30% antibacterial PET master batch is to join in the cortex with respect to 2%～6% of total fiber mass with antiseptic content, pure PET is as sandwich layer, Pi Yuxin is according to 1: the part by weight of 4-5 adds respectively in the double screw extruder, spins out the antibacterial PET fiber with skin-cored structure; Wherein spinning technology parameter is:
Sandwich layer: each is distinguished temperature and is respectively 280 ℃～290 ℃, 280 ℃～300 ℃, 280 ℃～300 ℃, 280 ℃～300 ℃; The measuring pump temperature is 280 ℃～297 ℃, and return bend temperature is 280 ℃～297 ℃; Screw speed is 41～55rpm; Pressure is 41～60 kilograms; For pump amount 5～8g/min;
Cortex: each is distinguished temperature and is respectively 280 ℃～290 ℃, 280 ℃～300 ℃, 280 ℃～300 ℃, 280 ℃～300 ℃; The measuring pump temperature is 280 ℃～297 ℃, and return bend temperature is 280 ℃～297 ℃, and spin manifold temperature is 290 ℃～310 ℃; Screw speed is 40～50rpm; Pressure is 30～40 kilograms; For pump amount 20～25g/min;
The technological parameter of drawtwister: draft temperature, temperature of heat plate are about 80 ℃, and hot plate temperature is about 160 ℃, and draw speed is 801～900m/min; Draw ratio: 4～5 times.
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