CN111253719B - Organic zinc antibacterial PET granules and preparation method thereof - Google Patents
Organic zinc antibacterial PET granules and preparation method thereof Download PDFInfo
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- CN111253719B CN111253719B CN201911130873.3A CN201911130873A CN111253719B CN 111253719 B CN111253719 B CN 111253719B CN 201911130873 A CN201911130873 A CN 201911130873A CN 111253719 B CN111253719 B CN 111253719B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- 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
-
- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
-
- 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
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0058—Biocides
Abstract
The invention discloses an organic zinc bacteriostatic PET grain and a preparation method thereof, wherein the organic zinc bacteriostatic PET grain is prepared by esterifying terephthalic acid, ethylene glycol and ethylene glycol titanium, and then polycondensing the esterified product with an antioxidant 1222, titanium dioxide and a pretreated organic zinc bacteriostatic agent S16. The bacteriostatic polyester fiber prepared by the organic zinc bacteriostatic PET granules has high bacteriostatic rate and lasting antibacterial effect, can keep the natural color of the fiber, is convenient for subsequent dyeing treatment, and has excellent ultraviolet resistance and mildew resistance.
Description
Technical Field
The invention belongs to the technical field of synthesis and processing of functional fibers, and particularly relates to an organic zinc antibacterial PET pellet and a preparation method thereof.
Background
With the enhancement of economic development and health consciousness of people, the requirements on the clothes do not meet the requirements of cold protection and warm keeping, and the comfort and the functionality of the clothes are more concerned. However, the clothes carry various germs in the wearing and using process, and peculiar smell is generated by absorbing sweat and the like secreted by a human body, so that people feel uncomfortable to wear and the health of the human body is affected. The antibacterial clothes play a key role in preventing bacteria breeding, eliminating peculiar smell and the like, and become an important branch of functional clothes research. In addition, the fields of medical treatment, health care, home furnishing, transportation and the like also put forward strong demands on the antibacterial performance of textiles, so that the antibacterial fiber products become one of the hot spots for developing functional fiber products.
At present, the antibacterial function of the fiber or the fabric is mainly realized by two methods, namely surface treatment and copolymerization or blending modification technology. The former is attached to the surface of the fiber or fabric by the adsorption or chemical bond between the antibacterial component and the surface of the fiber or fabric, thereby achieving the antibacterial effect. The method is simple and easy to implement and low in cost, but the product has poor washing resistance and wear resistance, poor lasting antibacterial performance, poor antibacterial agent heat resistance and easy generation of drug resistance. The copolymerization modification or blending modification is to add antibacterial components in the polymerization process to prepare antibacterial granules or add the antibacterial components into the polymer directly or after modification to prepare antibacterial master batches, and then prepare the antibacterial fiber by a melt spinning technology. This method is most widely used with inorganic antibacterial agents.
The antibacterial rate is one of the main test indexes for evaluating the antibacterial function of the antibacterial fiber or fabric. Silver-based antibacterial agents, which originally have excellent bactericidal and bacteriostatic activities, are the main representatives of inorganic antibacterial agents, and in recent years, with the development of technology, new inorganic antibacterial agents, such as copper-based and zinc-based antibacterial agents, have been developed. However, the copper-based bacteriostatic agent has the problem of fiber color, which affects the subsequent dyeing, so that the product application is limited, while the zinc-based bacteriostatic agent is mostly zinc oxide type, but the single nano zinc oxide has poor antibacterial performance, and the antibacterial performance needs to be improved by compounding other components of antibacterial agents. CN 102031584A discloses a preparation method of nano zinc oxide and titanium dioxide composite antibacterial polyester fiber. The antibacterial and deodorant polyester fiber prepared by the technical scheme disclosed in CN 102965760A is a broad-spectrum antibacterial agent compounded by zinc oxide whiskers and a silver antibacterial agent. The technical scheme disclosed in CN 108977925 a is to prepare a far infrared antibacterial polyester fiber by melt spinning with polyester as a substrate and composite filler a and composite filler B as additives, wherein the preparation method of the adopted composite antibacterial agent is complex, the addition amount of the inorganic filler is high, and the spinnability and the basic physical properties of the fiber are seriously affected.
In conclusion, the antibacterial and bacteriostatic fiber prepared in the prior art has the problems of poor antibacterial durability and heat resistance, poor compatibility between the antibacterial and bacteriostatic agent and fiber polyester, uneven distribution of antibacterial and bacteriostatic components, low continuous production yield especially for the production of special-shaped section fibers and the like. Therefore, while the basic physical properties of the fiber are maintained, the fiber product has a lasting antibacterial effect, and higher requirements are provided for the selection of antibacterial bacteriostatic agent components and the composite technology of the antibacterial components and the fiber.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an organic zinc bacteriostatic PET grain.
The invention also aims to provide a preparation method of the organic zinc bacteriostatic PET granules.
The technical scheme of the invention is as follows:
an organic zinc bacteriostatic PET grain is prepared by esterifying terephthalic acid, ethylene glycol and ethylene glycol titanium, and polycondensing with antioxidant 1222, titanium dioxide and pretreated organic zinc bacteriostatic agent S16;
the above-mentioned organozinc bacteriostatic agent S16 is preferably obtained from Shenyang antimicrobial technology Co., Ltdhttp：// microbe-free.cn/product0.html) The effective component is organic zinc.
In a preferred embodiment of the invention, the addition amount of the organic zinc in the organic zinc bacteriostatic PET granules is 500-1400 ppm.
In a preferred embodiment of the invention, the addition amount of the titanium glycol in the organic zinc bacteriostatic PET granules is 15-70 ppm.
In a preferred embodiment of the invention, the titanium dioxide is added in the organic zinc bacteriostatic PET pellets in an amount of 0 to 0.3 wt%.
In a preferred embodiment of the present invention, the antioxidant 1222 is added in the organic zinc bacteriostatic PET pellet in an amount of 1000-2500 ppm.
In a preferred embodiment of the present invention, the pretreatment is: and fully mixing the organic zinc bacteriostat S16, trimethyl phosphate and ethylene glycol to uniformly disperse the organic zinc bacteriostat S16 in the ethylene glycol.
More preferably, the addition amount of the trimethyl phosphate in the organic zinc bacteriostatic PET granules is 80-200 ppm.
The other technical scheme of the invention is as follows:
the preparation method of the organic zinc bacteriostatic PET granules comprises the following steps:
(1) weighing terephthalic acid, ethylene glycol and a catalyst titanium glycol with the acid-alcohol molar ratio of 1:1.15-1.4 according to the mass calculation of the organic zinc bacteriostatic PET granules theoretically produced, adding the terephthalic acid, the ethylene glycol and the catalyst titanium glycol into a reaction kettle for esterification reaction, wherein the temperature of the esterification reaction is 240-245 ℃, the pressure of the esterification reaction is micro-positive pressure of 0.01-0.03MPa, and the esterification is completed when the esterification rate reaches more than 98 percent to obtain an esterified substance;
(2) adding an antioxidant 1222, titanium dioxide and a pretreated organic zinc bacteriostatic agent S16 into the esterified product in sequence, maintaining the temperature of the esterified product at 208-215 ℃, balancing for 28-35min, then starting to heat and vacuumize, carrying out polycondensation reaction on the esterified product under the vacuum condition, stopping the reaction when the stirring current or the online viscosity value reaches a preset value, and extruding and pelletizing to obtain the organic zinc bacteriostatic PET pellets.
The invention has the beneficial effects that:
1. the bacteriostatic polyester fiber prepared by the organic zinc bacteriostatic PET granules has high bacteriostatic rate and lasting antibacterial effect, can keep the natural color of the fiber, is convenient for subsequent dyeing treatment, and has excellent ultraviolet resistance and mildew resistance.
2. The organic zinc antibacterial PET granules prepared by the invention have the advantages of simple preparation method and good thermal stability and spinnability.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
In the following examples, the pretreatment method for the organozinc bacteriostatic agent S16 (available from seiko shipwreck (shenyang) antimicrobial technologies ltd) was: fully diluting and fully stirring the mixture by using ethylene glycol, trimethyl phosphate serving as a stabilizer and an organic zinc bacteriostatic agent S16, and uniformly dispersing the organic zinc bacteriostatic agent S16 in the ethylene glycol.
In the following examples, the addition amounts of the organic zinc bacteriostat S16, trimethyl phosphate, the antioxidant 1222, titanium dioxide and titanium glycol are calculated according to the mass of the bacteriostasis PET theoretically produced, wherein the addition amounts are calculated according to effective components.
Example 1
Weighing terephthalic acid, ethylene glycol and 20ppm titanium glycol in a molar ratio of acid to alcohol of 1: 1.2 according to the mass calculation of bacteriostatic PET theoretically produced, adding the terephthalic acid, the ethylene glycol and the 20ppm titanium glycol into a reaction kettle for esterification reaction, wherein the temperature of the esterification reaction is 245 ℃, the pressure of the esterification reaction is micro-positive pressure of 0.02MPa, the esterification rate reaches more than 98 percent, adding 1500ppm of antioxidant 1222, 0.3 percent of titanium dioxide and 900ppm of pretreated organic zinc bacteriostatic agent S16 (containing 100ppm of stabilizer trimethyl phosphate) into the esterified substance in sequence, maintaining the temperature of the esterified substance at 208 DEG and 215 ℃, balancing for 30min, then starting to heat up and vacuumize, enabling the esterified substance to carry out polycondensation reaction at the reaction temperature of 275 ℃ and under the high vacuum condition of less than or equal to 80Pa, stopping the reaction after the stirring current or the online viscosity value reaches a preset value, and extruding and pelletizing to obtain the organic zinc bacteriostatic PET pellets.
And (2) putting the dried organic zinc antibacterial PET granules with the water content of below 30ppm into a granule cutting bin, heating and melting the granules from the intermediate bin to a spinning screw pump, feeding the granules into a spinning assembly through a filter and a melt pipeline, accurately metering and pressurizing the granules through a metering pump, extruding the granules from spinneret orifices of a spinneret plate, cooling the granules by blowing, oiling and winding the cooled granules to obtain pre-oriented yarns, and finally performing false twisting on the pre-oriented yarns to obtain the antibacterial polyester fibers. The temperature of the spinning assembly is 275 ℃, the spinning speed is 2900m/min, and spinneret orifices are cross-shaped; the first hot box temperature of the false twisting is 130 ℃, the second hot box temperature is 110 ℃, the drafting multiplying power is 1.75, and the processing speed is 750 m/min.
Example 2
Weighing terephthalic acid, ethylene glycol and 30ppm titanium glycol in a molar ratio of 1:1.15 of acid to alcohol, adding the terephthalic acid, the ethylene glycol and the 30ppm titanium glycol into a reaction kettle for esterification reaction, wherein the temperature of the esterification reaction is 244 ℃, the pressure of the esterification reaction is micro-positive pressure of 0.02MPa, the esterification rate reaches more than 98 percent, finishing the esterification, sequentially adding 1000ppm antioxidant 1222, 0.3 percent titanium dioxide and 500ppm pretreated organic zinc bacteriostat S16 (containing 100ppm stabilizer trimethyl phosphate) into the esterified product, maintaining the temperature of the esterified product at 208 DEG and 215 ℃, balancing for 30min, then starting heating and vacuumizing to perform polycondensation reaction on the esterified product at 275 ℃ and under high vacuum condition of less than or equal to 80Pa, stopping the reaction after the stirring current or online viscosity meter reaches a preset value, and extruding and granulating to obtain the organic zinc bacteriostatic PET granules.
And (2) putting the dried organic zinc antibacterial PET granules with the water content of below 30ppm into a granule cutting bin, heating and melting the granules from the intermediate bin to a spinning screw pump, feeding the granules into a spinning assembly through a filter and a melt pipeline, accurately metering and pressurizing the granules through a metering pump, extruding the granules from spinneret orifices of a spinneret plate, cooling the granules by blowing, oiling and winding the cooled granules to obtain pre-oriented yarns, and finally performing false twisting on the pre-oriented yarns to obtain the antibacterial polyester fibers. The temperature of the spinning assembly is 278 ℃, the spinning speed is 2900m/min, and the spinneret orifices are cross; the first hot box temperature of the false twisting is 130 ℃, the second hot box temperature is 110 ℃, the drafting multiplying power is 1.78, and the processing speed is 800 m/min.
Example 3
Weighing terephthalic acid, ethylene glycol and 50ppm titanium glycol in a molar ratio of 1: 1.4 of acid to alcohol, adding the terephthalic acid, the ethylene glycol and the 50ppm titanium glycol into a reaction kettle for esterification reaction, wherein the temperature of the esterification reaction is 242 ℃, the pressure of the esterification reaction is 0.02MPa of micro positive pressure, the esterification rate reaches more than 98 percent, completing the esterification, sequentially adding 2000ppm antioxidant 1222 and 900ppm pretreated organic zinc bacteriostat S16 (containing 150ppm stabilizer trimethyl phosphate) into the esterified product, maintaining the temperature of the esterified product at 208 DEG and 215 ℃, starting to heat and vacuumize after balancing for 30min, enabling the esterified product to carry out polycondensation reaction at the reaction temperature of 275 ℃ and the high vacuum condition of less than or equal to 80Pa, stopping the reaction after the stirring current or the online viscosity value reaches the preset value, and extruding and pelletizing to obtain the organic zinc bacteriostasis PET pellets.
And (2) putting the dried organic zinc antibacterial PET granules with the water content of below 30ppm into a granule cutting bin, heating and melting the granules from the intermediate bin to a spinning screw pump, feeding the granules into a spinning assembly through a filter and a melt pipeline, accurately metering and pressurizing the granules through a metering pump, extruding the granules from spinneret orifices of a spinneret plate, cooling the granules by blowing, oiling and winding the cooled granules to obtain pre-oriented yarns, and finally performing false twisting on the pre-oriented yarns to obtain the antibacterial polyester fibers. The temperature of the spinning assembly is 275 ℃, the spinning speed is 2700m/min, and the spinneret orifices are circular; the first hot box temperature of the false twisting is 130 ℃, the second hot box temperature is 110 ℃, the drafting multiplying power is 1.75, and the processing speed is 750 m/min.
Example 4
Weighing terephthalic acid, ethylene glycol and 70ppm titanium glycol in a molar ratio of 1:1.15 of acid to alcohol, adding the terephthalic acid, the ethylene glycol and the 70ppm titanium glycol into a reaction kettle for esterification reaction, wherein the temperature of the esterification reaction is 240 ℃, the pressure of the esterification reaction is 0.02MPa of micro positive pressure, the esterification rate reaches more than 98 percent, completing the esterification, sequentially adding 1500ppm of antioxidant 1222, 0.3 percent of titanium dioxide and 1400ppm of pretreated organic zinc bacteriostat S16 (containing 150ppm of trimethyl phosphate), maintaining the temperature of the esterified product at 208-215 ℃, balancing for 30min, then starting heating and vacuumizing to perform polycondensation reaction on the esterified product at the reaction temperature of 270 ℃ and under the high vacuum condition of less than or equal to 80Pa, stopping the reaction after the stirring current or the online viscosity meter reaches a preset value, and extruding and granulating to obtain the organic zinc bacteriostatic PET granules.
And (2) putting the dried organic zinc antibacterial PET granules with the water content of below 30ppm into a granule cutting bin, heating and melting the granules from the intermediate bin to a spinning screw pump, feeding the granules into a spinning assembly through a filter and a melt pipeline, accurately metering and pressurizing the granules through a metering pump, extruding the granules from spinneret orifices of a spinneret plate, cooling the granules by blowing, oiling and winding the cooled granules to obtain pre-oriented yarns, and finally performing false twisting on the pre-oriented yarns to obtain the antibacterial polyester fibers. The temperature of the spinning assembly is 270 ℃, the spinning speed is 2800m/min, and the spinneret orifices are circular; the first hot box temperature of the false twisting is 130 ℃, the second hot box temperature is 110 ℃, the drafting multiplying power is 1.75, and the processing speed is 800 m/min.
Example 5
The detection method of the high-efficiency bacteriostatic polyester fiber and fabric prepared in the above embodiments is described as follows:
1. the fiber antibacterial performance test is carried out according to the national standard GB/T20944.3-2008.
2. The fiber mildew resistance test is carried out according to the national standard GB/T24346-2009.
3. The UV resistance test of the fiber fabric is carried out according to the standard AATCC 183-2014.
The main performance test indexes of the high-efficiency antibacterial polyester fibers and the high-efficiency antibacterial polyester fabrics prepared in the examples 1 to 4 are shown in tables 1 to 3.
TABLE 1. bacteriostasis rate of 50 times of water washing for high-efficiency bacteriostasis polyester fiber fabrics prepared in examples 1-4
TABLE 2 mildew resistance of the highly effective bacteriostatic polyester fibers prepared in examples 1-4
TABLE 3. examples 1-4 preparation of highly effective antibacterial polyester fiber fabrics with anti-UV property in dry and wet states
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (8)
1. An organic zinc antibacterial PET grain, which is characterized in that: is prepared by esterification of terephthalic acid, ethylene glycol and titanium glycol, and polycondensation of the esterification product, antioxidant 1222, titanium dioxide and pretreated organic zinc bacteriostatic agent S16;
the effective component of the organic zinc bacteriostatic agent S16 is organic zinc.
2. The organic zinc bacteriostatic PET pellet as claimed in claim 1, wherein: the addition amount of the organic zinc in the organic zinc bacteriostatic PET grain is 500-1400 ppm.
3. The organic zinc bacteriostatic PET pellet as claimed in claim 1, wherein: the addition amount of the ethylene glycol titanium in the organic zinc bacteriostatic PET grain is 15-70 ppm.
4. The organic zinc bacteriostatic PET pellet as claimed in claim 1, wherein: the addition amount of the titanium dioxide in the organic zinc bacteriostatic PET granules is 0-0.3 wt%.
5. The organic zinc bacteriostatic PET pellet as claimed in claim 1, wherein: the addition amount of the antioxidant 1222 in the organic zinc bacteriostatic PET granules is 1000-2500 ppm.
6. The organic zinc bacteriostatic PET pellet as claimed in claim 1, wherein: the pretreatment comprises the following steps: and fully mixing the organic zinc bacteriostat S16, trimethyl phosphate and ethylene glycol to uniformly disperse the organic zinc bacteriostat S16 in the ethylene glycol.
7. The organic zinc bacteriostatic PET pellet as claimed in claim 6, wherein: the addition amount of the trimethyl phosphate in the organic zinc bacteriostatic PET granules is 80-200 ppm.
8. The method for preparing the organic zinc bacteriostatic PET granules according to any one of claims 1 to 7, which is characterized by comprising the following steps: the method comprises the following steps:
(1) weighing terephthalic acid, ethylene glycol and a catalyst titanium glycol with the acid-alcohol molar ratio of 1:1.15-1.4 according to the mass calculation of the organic zinc bacteriostatic PET granules theoretically produced, adding the terephthalic acid, the ethylene glycol and the catalyst titanium glycol into a reaction kettle for esterification reaction, wherein the temperature of the esterification reaction is 240-245 ℃, the pressure of the esterification reaction is micro-positive pressure of 0.01-0.03MPa, and the esterification is completed when the esterification rate reaches more than 98 percent to obtain an esterified substance;
(2) adding an antioxidant 1222, titanium dioxide and a pretreated organic zinc bacteriostatic agent S16 into the esterified product in sequence, maintaining the temperature of the esterified product at 208-215 ℃, balancing for 28-35min, then starting to heat and vacuumize, carrying out polycondensation reaction on the esterified product under the vacuum condition, stopping the reaction when the stirring current or the online viscosity value reaches a preset value, and extruding and pelletizing to obtain the organic zinc bacteriostatic PET pellets.
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| CN115637504A (en) * | 2021-07-20 | 2023-01-24 | 中国石油天然气股份有限公司 | Antibacterial DTY fiber and method for continuously producing antibacterial DTY fiber |
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| CN1182176C (en) * | 2002-12-27 | 2004-12-29 | 济南正昊化纤新材料有限公司 | Process for preparing antibiotic polyester |
| CN101238817B (en) * | 2008-03-06 | 2011-09-14 | 刘燕平 | Bacteriostat, far-infrared ray emitting agent, mother particle, fiber and manufacturing method thereof |
| EP2294260B1 (en) * | 2008-06-30 | 2016-11-02 | Bar-Ilan University | Sonochemical coating of textiles with metal oxide nanoparticles for antimicrobial fabrics |
| CN107761188A (en) * | 2017-11-24 | 2018-03-06 | 陕西盛迈石油有限公司 | The preparation method of copper zinc composite antibacterial polyester fiber |
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