CN111253718B - Organic zinc antibacterial master batch for spinning and preparation method thereof - Google Patents
Organic zinc antibacterial master batch for spinning and preparation method thereof Download PDFInfo
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- CN111253718B CN111253718B CN201911126715.0A CN201911126715A CN111253718B CN 111253718 B CN111253718 B CN 111253718B CN 201911126715 A CN201911126715 A CN 201911126715A CN 111253718 B CN111253718 B CN 111253718B
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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
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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
- D01F6/88—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
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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
- 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
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- 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
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses an organic zinc bacteriostatic master batch for spinning and a preparation method thereof, wherein the organic zinc bacteriostatic master batch comprises the following raw material components: 70-92 parts of fiber-grade PBT powder, 165-30 parts of organic zinc bacteriostatic agent S, 0.5-2.5 parts of zinc stearate, 0.1-0.5 part of trimethyl phosphate, 12220.1-0.5 part of antioxidant and a proper amount of ethylene glycol. The organic zinc bacteriostatic master batch for spinning has the advantages of simple preparation method, high bacteriostatic rate, lasting antibacterial effect, good safety, and good thermal stability and spinnability when used for preparing bacteriostatic fibers; the organic zinc bacteriostatic master batch for spinning can keep the natural color of the prepared bacteriostatic fiber, and is convenient for the subsequent dyeing treatment.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to an organic zinc bacteriostatic master batch for spinning and a preparation method thereof.
Background
With the enhancement of economic development and health consciousness of people, strong demands are put forward on functional textiles such as antibacterial, mildewproof, ultraviolet-resistant, far infrared and the like in the fields of medical treatment, health care, home furnishing, traffic and the like, and especially the antibacterial and mildewproof textiles become one of hot spots of functional product development in recent years. The antibacterial function of the antibacterial textile is mainly realized by two methods, namely surface treatment and copolymerization or blending modification technology.
The blending modification is to add the antibacterial component into the polymer directly or after modification to prepare antibacterial master batch, and then prepare the antibacterial fiber by a melt spinning technology. The method has the advantages of wide application of inorganic antibacterial agent, no disadvantages of surface treatment and poor antibacterial durability and heat resistance of organic antibacterial agent, and flexible and convenient addition. But the compatibility of the inorganic antibacterial agent and fiber polyester is poor, the distribution of antibacterial components is uneven, the continuous production is low in the production yield of the special-shaped cross-section fiber, the hand feeling of the prepared fabric is rough, and the like. Therefore, the basic physical properties of the fiber are maintained, and meanwhile, the fiber product has a durable antibacterial effect, and higher requirements are provided for selection of antibacterial agent components and addition modes.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an organic zinc bacteriostatic master batch for spinning.
The invention also aims to provide a preparation method of the organic zinc bacteriostatic master batch for spinning.
The technical scheme of the invention is as follows:
an organic zinc bacteriostatic master batch for spinning comprises the following raw material components: 70-92 parts of fiber-grade PBT powder, 165-30 parts of organic zinc bacteriostatic agent S, 0.5-2.5 parts of zinc stearate, 0.1-0.5 part of trimethyl phosphate, 12220.1-0.5 part of antioxidant and a proper amount of ethylene glycol;
the intrinsic viscosity is 0.72-0.80dL/g, the melting point is 224-225 ℃, the chroma b value is 3.5-4.5, the chroma L value is 85-88, and the bacteriostasis rate of the product on staphylococcus aureus, escherichia coli and candida albicans is more than or equal to 99 percent.
In a preferred embodiment of the invention, the intrinsic viscosity of the fiber-grade PBT powder is 0.88-1.0 dL/g.
In a preferred embodiment of the invention, the molar ratio of the ethylene glycol to the organic zinc in the organic zinc bacteriostatic agent S16 is 2-2.2: 1.
The other technical scheme of the invention is as follows:
the preparation method of the organic zinc bacteriostatic master batch for spinning comprises the following steps:
(1) mixing and reacting the organic zinc bacteriostat S16, ethylene glycol, trimethyl phosphate and an antioxidant 1222 to prepare an organic zinc pretreatment solution;
(2) putting the fiber-grade PBT powder and zinc stearate into a high-speed mixing roll, and fully stirring and mixing for 2-4min at the rotating speed of 500-1500 rpm;
(3) adding the organic zinc pretreatment solution into the material obtained in the step (2), and continuously stirring and mixing for 4-6min in a high-speed mixing roll at the rotating speed of 500-1500 rpm;
(4) and (4) feeding the material obtained in the step (3) into a vacuum double-screw extruder, and performing extrusion processing and granulation to obtain the organic zinc bacteriostatic master batch for spinning.
In a preferred embodiment of the present invention, the step (1) is: adding the organic zinc bacteriostat S16 and ethylene glycol into an enamel reaction kettle, fully stirring and mixing, adding trimethyl phosphate and antioxidant 1222, heating to 145-155 ℃, controlling the temperature of a separation tower to be 58-62 ℃, reacting for 25-35min, and cooling to room temperature to obtain the organic zinc pretreatment solution.
In a preferred embodiment of the present invention, the rotation speed in the steps (2) and (3) is 700 and 1000 rpm.
In a preferred embodiment of the invention, the length-diameter ratio of the screw of the vacuum double-screw extruder is 39-42:1, the processing temperature of the screw is 220-265 ℃, and the rotating speed of the screw is 200-500 rpm.
The invention has the beneficial effects that:
1. the preparation method of the organic zinc bacteriostatic master batch for spinning is simple.
2. The organic zinc bacteriostatic master batch for spinning has high bacteriostatic rate, lasting antibacterial effect and good safety.
3. The organic zinc bacteriostatic master batch for spinning is used for preparing bacteriostatic fibers, and has good thermal stability and spinnability.
4. The organic zinc bacteriostatic master batch for spinning can keep the natural color of the prepared bacteriostatic fiber, and is convenient for the subsequent dyeing treatment.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
Example 1
(1) An organozinc bacteriostatic agent S16 (available from seiko (shenyang) antimicrobial technologies ltd,http:// microbe-free.cn/product0.html) Adding 7 parts by weight of glycol and glycol (the molar ratio of the glycol to the organic zinc in the organic zinc bacteriostatic agent S16 is 2.1: 1) into an enamel reaction kettle, fully stirring and mixing, adding 0.2 part by weight of trimethyl phosphate and 0.1 part by weight of antioxidant 1222, heating to 150 ℃, controlling the temperature of a separation tower to be 60 ℃, reacting for 30min, and cooling to room temperature to obtain an organic zinc pretreatment solution;
(2) putting 92 parts by weight of fiber-grade PBT powder with the intrinsic viscosity of 0.95dL/g and 0.7 part by weight of zinc stearate into a high-speed mixing roll, and fully stirring and mixing for 3min at the rotating speed of 750 rpm;
(3) adding the organic zinc pretreatment solution into the material obtained in the step (2), and continuously stirring and mixing for 5min in a high-speed mixing roll at the rotating speed of 750 rpm;
(4) feeding the material obtained in the step (3) into a vacuum double-screw extruder (the length-diameter ratio of a screw is 40: 1, the processing temperature of the screw is 220-;
the organic zinc bacteriostatic master batch for spinning prepared by the embodiment has the particle size of 3mm, the length of 3mm, the intrinsic viscosity of 0.75dL/g, the melting point of 224 ℃, the chroma b value of 4.5 and the chroma L value of 85, and the bacteriostatic rates on staphylococcus aureus, escherichia coli and candida albicans are respectively more than or equal to 99%, and the organic zinc bacteriostatic master batch has good filterability and spinnability.
Example 2
(1) Adding 15 parts by weight of organic zinc bacteriostat S16 (purchased from Shenyang antimicrobial science and technology Co., Ltd.) and ethylene glycol (the molar ratio of the ethylene glycol to the organic zinc in the organic zinc bacteriostat S16 is 2.1: 1) into an enamel reaction kettle, fully stirring and mixing, adding 0.4 part by weight of trimethyl phosphate and 0.4 part by weight of antioxidant 1222, heating to 150 ℃, controlling the temperature of a separation tower to be 60 ℃, reacting for 30min, and cooling to room temperature to prepare organic zinc pretreatment liquid;
(2) putting 82 parts by weight of fiber-grade PBT powder with the intrinsic viscosity of 1.0dL/g and 2.2 parts by weight of zinc stearate into a high-speed mixing roll, and fully stirring and mixing for 3min at the rotating speed of 750 rpm;
(3) adding the organic zinc pretreatment solution into the material obtained in the step (2), and continuously stirring and mixing for 5min in a high-speed mixing roll at the rotating speed of 750 rpm;
(4) feeding the material obtained in the step (3) into a vacuum double-screw extruder (the length-diameter ratio of a screw is 40: 1, the processing temperature of the screw is 220-;
the organic zinc bacteriostatic master batch for spinning prepared by the embodiment has the particle size of 3mm, the length of 3mm, the intrinsic viscosity of 0.80dL/g, the melting point of 225 ℃, the chroma b value of 3.7 and the chroma L value of 87, and the bacteriostatic rates on staphylococcus aureus, escherichia coli and candida albicans are respectively more than or equal to 99%, and the organic zinc bacteriostatic master batch for spinning has good filterability and spinnability.
Example 3
(1) Adding 25 parts by weight of organic zinc bacteriostat S16 (purchased from Shenyang antimicrobial science and technology Co., Ltd.) and ethylene glycol (the molar ratio of the ethylene glycol to the organic zinc in the organic zinc bacteriostat S16 is 2.1: 1) into an enamel reaction kettle, fully stirring and mixing, adding 0.4 part by weight of trimethyl phosphate and 0.2 part by weight of antioxidant 1222, heating to 150 ℃, controlling the temperature of a separation tower to be 60 ℃, reacting for 30min, and cooling to room temperature to prepare organic zinc pretreatment liquid;
(2) putting 72 parts by weight of fiber-grade PBT powder with the intrinsic viscosity of 0.88dL/g and 2.4 parts by weight of zinc stearate into a high-speed mixing roll, and fully stirring and mixing for 3min at the rotating speed of 950 rpm;
(3) adding the organic zinc pretreatment solution into the material obtained in the step (2), and continuously stirring and mixing for 5min in a high-speed mixing roll at the rotating speed of 950 rpm;
(4) feeding the material obtained in the step (3) into a vacuum double-screw extruder (the length-diameter ratio of a screw is 40: 1, the processing temperature of the screw is 220-;
the organic zinc bacteriostatic master batch for spinning prepared by the embodiment has the particle size of 3mm, the length of 3mm, the intrinsic viscosity of 0.72dL/g, the melting point of 224 ℃, the chroma b value of 3.6 and the chroma L value of 85, and the bacteriostatic rates on staphylococcus aureus, escherichia coli and candida albicans are respectively more than or equal to 99%, and the organic zinc bacteriostatic master batch has good filterability and spinnability.
The performance detection method of the spinning organic zinc antibacterial master batch prepared in the above embodiments is described as follows:
1. the intrinsic viscosity, the melting point and the chromaticity of the antibacterial master batch are tested according to the national standard GB/T14190-2008, wherein the intrinsic viscosity solvent adopts phenol/1, 1,2, 2-tetrachloroethane with the mass ratio of 60:40, and the melting point test adopts differential scanning calorimetry.
2. The antibacterial performance test of the antibacterial master batch is carried out according to the national standard GB/T31402-2015.
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 (7)
1. An organic zinc antibacterial master batch for spinning is characterized in that: comprises the following raw material components: 70-92 parts of fiber-grade PBT powder, 165-30 parts of organic zinc bacteriostatic agent S, 0.5-2.5 parts of zinc stearate, 0.1-0.5 part of trimethyl phosphate, 12220.1-0.5 part of antioxidant and a proper amount of ethylene glycol;
the intrinsic viscosity is 0.72-0.80dL/g, the melting point is 224-225 ℃, the chroma b value is 3.5-4.5, the chroma L value is 85-88, and the bacteriostasis rate of the product on staphylococcus aureus, escherichia coli and candida albicans is more than or equal to 99 percent;
the testing of the intrinsic viscosity, the melting point, the chromaticity b and the chromaticity L is carried out according to the national standard GB/T14190-2008, wherein the intrinsic viscosity solvent adopts the mass ratio of phenol to 1,1,2, 2-tetrachloroethane of 60:40, and the melting point testing adopts differential scanning calorimetry;
the bacteriostasis rate is tested according to the national standard GB/T31402-2015.
2. The spinning organic zinc bacteriostatic master batch of claim 1, which is characterized in that: the intrinsic viscosity of the fiber-grade PBT powder is 0.88-1.0 dL/g.
3. The spinning organic zinc bacteriostatic master batch of claim 1, which is characterized in that: the molar ratio of the ethylene glycol to the organic zinc in the organic zinc bacteriostatic agent S16 is 2-2.2: 1.
4. The preparation method of the spinning organic zinc bacteriostatic master batch of any one of claims 1 to 3, which is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing and reacting the organic zinc bacteriostat S16, ethylene glycol, trimethyl phosphate and an antioxidant 1222 to prepare an organic zinc pretreatment solution;
(2) putting the fiber-grade PBT powder and zinc stearate into a high-speed mixing roll, and fully stirring and mixing for 2-4min at the rotating speed of 500-1500 rpm;
(3) adding the organic zinc pretreatment solution into the material obtained in the step (2), and continuously stirring and mixing for 4-6min in a high-speed mixing roll at the rotating speed of 500-1500 rpm;
(4) and (4) feeding the material obtained in the step (3) into a vacuum double-screw extruder, and performing extrusion processing and granulation to obtain the organic zinc bacteriostatic master batch for spinning.
5. The method of claim 4, wherein: the step (1) is as follows: adding the organic zinc bacteriostat S16 and ethylene glycol into an enamel reaction kettle, fully stirring and mixing, adding trimethyl phosphate and antioxidant 1222, heating to 145-155 ℃, controlling the temperature of a separation tower to be 58-62 ℃, reacting for 25-35min, and cooling to room temperature to obtain the organic zinc pretreatment solution.
6. The method of claim 4, wherein: the rotation speed in the steps (2) and (3) is 700 and 1000 rpm.
7. The method of claim 4, wherein: the length-diameter ratio of the screw of the vacuum double-screw extruder is 39-42:1, the processing temperature of the screw is 220-265 ℃, and the rotating speed of the screw is 200-500 rpm.
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| CN201911126715.0A CN111253718B (en) | 2019-11-18 | 2019-11-18 | Organic zinc antibacterial master batch for spinning and preparation method thereof |
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| CN111253718B true CN111253718B (en) | 2022-03-15 |
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| US20050019572A1 (en) * | 2003-07-22 | 2005-01-27 | Shin-Hsin Chang | Manufacturing method for polymer chips containing metal or metal oxide nanoparticles component |
| 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 |
| CN102838852A (en) * | 2012-09-26 | 2012-12-26 | 上海瀚氏模具成型有限公司 | PBT (Polybutylece Terephthalate) plastic used for automotive interiors and preparation method thereof |
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