CN117547922A - Negative oxygen ion air purification material and preparation process thereof - Google Patents

Negative oxygen ion air purification material and preparation process thereof Download PDF

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Publication number
CN117547922A
CN117547922A CN202311553914.6A CN202311553914A CN117547922A CN 117547922 A CN117547922 A CN 117547922A CN 202311553914 A CN202311553914 A CN 202311553914A CN 117547922 A CN117547922 A CN 117547922A
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fiber
solution
negative oxygen
tourmaline powder
oxygen ion
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葛玲
袁燕
陈凤
陈永兵
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Violet Home Textile Technology Co Ltd
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Violet Home Textile Technology Co Ltd
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Priority to CN202311553914.6A priority Critical patent/CN117547922A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/68Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03Polysaccharides or derivatives thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03Polysaccharides or derivatives thereof
    • D06M15/11Starch or derivatives thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2253/00Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/25Coated, impregnated or composite adsorbents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/91Bacteria; Microorganisms
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention provides a negative oxygen ion air purification material and a preparation process thereof, and relates to the field of textile fibers. The method comprises the following steps: mixing nano tourmaline powder with graphene oxide aqueous solution, performing ultrasonic dispersion, adding urea into cellulose solution, uniformly stirring, adding epichlorohydrin, and stirring for 1-2h; adding the mixture A and the water-soluble polyethylene glycol solution at the same time, and stirring for 1-2h to obtain spinning solution; spinning and forming to obtain fiber yarns; adding nano tourmaline powder into an ethanol water solution, adding a double bond silane coupling agent and beta-cyclodextrin, and adding a starch water solution to obtain a mixture B; placing the fiber filaments in the mixture B, standing for 15-18h at 1-2 ℃, and vacuum drying at low temperature to obtain modified fiber filaments; taking modified fiber yarns as core materials and plant fibers as outer fiber layers, and spinning to obtain core-spun yarns; soaking the core spun yarn in water for several times, and naturally drying. The nano tourmaline powder of the material is not easy to fall off, has strong binding strength with fiber and has strong washing fastness.

Description

Negative oxygen ion air purification material and preparation process thereof
Technical Field
The invention relates to the field of textile fibers, in particular to a negative oxygen ion air purification material and a preparation process thereof.
Background
The negative oxygen ion refers to the sum of single gas molecules and hydrogen ion groups with negative charges, has the effect of purifying air, can decompose pollutants such as formaldehyde, toluene and the like in the air, and can be combined with bacteria to change the structure of the bacteria, so that the sterilizing effect is achieved.
Negative oxygen ions are introduced into the fabric, and can release a certain amount of negative oxygen ions into the surrounding environment, so that the effect of purifying air is achieved. At present, two modes from the fabric to the addition of negative oxygen ions mainly exist, namely, the negative oxygen ion generating substances (such as tourmaline powder and the like) are directly coated, soaked and wrapped on the surface of the fiber or the fabric, so that the negative oxygen ions can be released after the fiber or the fabric is manufactured into a product. In the other process, the negative oxygen ion generating substance is mixed with the fiber raw material and then spun into fiber filaments through the working procedures of spinning and the like, so that the fibers or fabrics can release negative oxygen ions.
The patent 202210831552.1 discloses a negative ion heating graphene modified fine denier fiber and a preparation method thereof, wherein graphene oxide is utilized to modify cotton linter fibers to obtain fiber blanks, the fiber blanks and tourmaline slurry are dispersed and mixed, and the fibers capable of releasing negative oxygen ions can be obtained after washing, oiling and other operations.
Patent 202210425846.4 discloses a fabric containing negative oxygen ions and a production process thereof, wherein negative ion powder is added into a fabric treating agent, and then the fabric is treated by the treating agent, so that the fabric capable of releasing the negative oxygen ions can be obtained.
Patent 202011590445.1 discloses a method for producing anion-generating fiber, which comprises mixing tourmaline, medical stone, titanium pigment, alumina mixed powder with organic solvent, coupling agent, dispersing agent, etc., and then carrying out blending granulation and wet spinning to obtain the anion fiber.
The currently disclosed fiber or fabric capable of releasing negative oxygen ions has low binding fastness between tourmaline and fiber/fabric, is easy to fall off after washing, and cannot release negative oxygen ions for a long time.
Disclosure of Invention
The invention aims to provide a negative oxygen ion air purification material, wherein a part of nano tourmaline powder is attached to the inside of an inner layer fiber, a part of nano tourmaline powder is arranged on the surface of the fiber, the nano tourmaline powder is not easy to fall off, and the bonding fastness with the fiber is strong.
The invention also aims to provide a preparation method of the negative oxygen ion air purification material, and the core spun yarn fiber prepared by the method can release negative oxygen ions for a long time.
The invention solves the technical problems by adopting the following technical scheme.
In one aspect, the embodiment of the invention provides a preparation process of a negative oxygen ion air purification material, which comprises the following steps:
s1: mixing nano tourmaline powder with graphene oxide aqueous solution, and performing ultrasonic dispersion to obtain a mixture A; adding urea into the cellulose solution, uniformly stirring, adding epichlorohydrin, and stirring for 1-2h; adding the mixture A and the water-soluble polyethylene glycol solution at the same time, and stirring for 1-2h to obtain spinning solution; spinning and forming the spinning solution to obtain fiber yarns;
s2: adding nano tourmaline powder into an ethanol water solution, performing ultrasonic dispersion, adding a double bond silane coupling agent and beta-cyclodextrin, uniformly stirring, adding a starch water solution, and performing ultrasonic dispersion to obtain a mixture B; placing the fiber yarn prepared in the step S2 into the mixture B, standing for 15-18h at 1-2 ℃, and carrying out low-temperature vacuum drying to obtain modified fiber yarn;
s3: taking the modified fiber yarn prepared in the step S2 as a core material, taking plant fiber as an outer fiber layer, and spinning to obtain core spun yarn;
s4: soaking the core spun yarn in water for multiple times, and naturally airing.
The modified fiber loaded with nano tourmaline powder is used as a core material, the plant fiber is used as an outer layer, the spun core yarn is obtained, and part of starch on the surface of the inner layer fiber is removed after washing, so that a certain pore is formed between the inner layer fiber and the outer layer, on one hand, the hygroscopicity and adsorptivity of the fiber can be improved, and the pore can be used for adsorbing pollutants in the air.
In some embodiments of the invention, the cellulose solution is prepared by the steps of: pulverizing bamboo fiber, soaking in sodium hydroxide solution, heating to 45-55deg.C, adding carbon disulfide into the reaction system at the temperature, stirring, and maintaining the temperature for 5-6 hr to obtain cellulose solution.
In some embodiments of the invention, further comprising: in the heat preservation process, inert gas is introduced into the reaction system through an aeration device. In the process of preparing the cellulose solution, through aeration treatment, the fiber can be fluffy, micropores are formed on the fiber, space is provided for the subsequent loading of tourmaline powder, and cyclodextrin molecules are tightly combined with fiber yarns.
In some embodiments of the invention, the double bond silane coupling agent is gamma-methacryloxypropyl trimethoxysilane, vinyl triethoxysilane, or vinyl trimethoxysilane. The double bond coupling agent can provide double bond functional groups, can be used as a dispersing agent in the reaction process, and can avoid agglomeration of nano tourmaline powder.
In some embodiments of the invention, in step S2, further comprising, in mixture B, adding an antimicrobial agent;
wherein the antibacterial agent comprises the following raw materials in parts by weight: 10-20 parts of chitosan quaternary ammonium salt, 5-10 parts of titanium dioxide and 0.5-1 part of potassium persulfate.
In the step S2, an antibacterial agent is added, and chitosan quaternary ammonium salt in the antibacterial agent has certain antibacterial property, and titanium dioxide can absorb ultraviolet rays, so that the antibacterial aging of the quaternary ammonium salt is prolonged; and the double bond silane coupling agent can graft and modify the titanium dioxide, so that the titanium dioxide has reactive double bond groups, the titanium dioxide can be combined on the fiber through reaction, and then the molecular chain can be wound on the fiber in the ultrasonic dispersion process of the chitosan quaternary ammonium salt, so that the load fastness is improved.
In some embodiments of the invention, the plant fibers are one or more of cotton fibers, bamboo fibers, ramie fibers, and sisal fibers.
In some embodiments of the present invention, in the step S2, the mass ratio of the nano tourmaline powder, the double bond silane coupling agent and the β -cyclodextrin is 1: (0.1-0.5): (1.5-3). And a small amount of silane coupling agent is added, so that the nano tourmaline powder can be dispersed and used as a bridge of inorganic and organic molecules, and the cyclodextrin can be used for coating the nano tourmaline powder more easily. And the excessive cyclodextrin is added, so that most of nano tourmaline powder can be coated, the excessive cyclodextrin can also increase the viscosity of a solution system, and the coating is more easily loaded on the fiber.
In some embodiments of the present invention, in the step S1, a mass ratio of the nano tourmaline powder to the water-soluble polyethylene glycol is 1: (0.5-1). The addition of a small amount of polyethylene glycol can increase the number of hydroxyl groups on the fiber, namely, the fiber is hydroxylated, and the hydroxyl groups can form hydrogen bonds with stronger molecular force with substances such as cyclodextrin and the like, so that the bonding strength is improved.
In some embodiments of the present invention, in the step S2, the mass ratio of nano tourmaline powder to starch is 1: (2-5).
On the other hand, the embodiment of the invention provides a negative oxygen ion air purification material which is prepared by the preparation process.
Compared with the prior art, the embodiment of the invention has at least the following advantages or beneficial effects:
in the application, nano tourmaline powder is loaded on the fibers in different modes, and as tourmaline can release anions, the anions in the air can play a role in purifying the air, fabrics made of the fibers, such as curtains and the like, can release anions continuously, and the effect of purifying the indoor air is achieved.
In the application, graphene oxide is utilized to modify nano tourmaline powder, then the nano tourmaline powder is mixed with cellulose solution, water-soluble polyethylene glycol is matched, fiber filaments are obtained after spinning and forming, polyethylene glycol, graphene oxide and cellulose form a crosslinked network structure, nano tourmaline powder is embedded in the network structure, on one hand, the fastness of tourmaline powder and a matrix can be enhanced, on the other hand, graphene molecules and cellulose molecules are mutually crosslinked and wound, and the elasticity and strength of the fiber can be enhanced. Second, the hydroxyl groups of the polyethylene glycol in the filament can serve as the active sites for subsequent reactions.
On the other hand, the double bond silane coupling agent and the beta-cyclodextrin are added into the nano tourmaline powder, the nano tourmaline powder is wrapped inside by utilizing the wrapping property of the beta-cyclodextrin, the double bond silane coupling agent can also play a role in dispersing, the agglomeration of the nano tourmaline powder can be avoided in the reaction process, and the formation of a wrapper with smaller particle size is promoted; by utilizing the adhesion effect of starch, the cyclodextrin and the double bond silane coupling agent are more easily attached to the fiber, and in the low-temperature soaking process, the cyclodextrin can form a hydrogen bond with a hydroxyl group on the fiber, so that the cyclodextrin can wrap nano tourmaline powder on the fiber in situ, and the firmness of the nano tourmaline powder and the fiber is improved.
In conclusion, the nano tourmaline powder is loaded twice, so that the load capacity of the nano tourmaline powder can be improved, the load strength can be improved, the fabric is more resistant to water washing, the retention time of the tourmaline powder on the fabric is longer, and the ageing of releasing negative oxygen ions by the fabric is longer.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other. The present invention will be described in detail with reference to specific examples.
Example 1
S1, crushing bamboo fibers to 1-2cm, soaking the bamboo fibers in a sodium hydroxide solution with the mass fraction of 2% for 30min, heating the system to 55 ℃, adding carbon disulfide liquid into a reaction system at the temperature, uniformly stirring, preserving the heat for 6h, and introducing nitrogen into the reaction system through an aeration device in the heat preservation process to obtain a cellulose solution; mixing nano tourmaline powder with graphene oxide aqueous solution, and performing ultrasonic dispersion to obtain a mixture A; adding urea into the cellulose solution, uniformly stirring, adding epichlorohydrin, and stirring for 2 hours; adding the mixture A and the water-soluble polyethylene glycol solution at the same time, and stirring for 2 hours to obtain spinning solution; filtering and defoamating the spinning solution, and adding the filtered and defoamed spinning solution into a spinning bath with the temperature of 40 ℃ for spinning and forming to obtain fiber yarns; wherein the spinning bath comprises: 80g/L of sulfuric acid, 150g/L of sodium sulfate and 5g/L of zinc sulfate; the mass ratio of the nano tourmaline powder to the water-soluble polyethylene glycol is 1:0.5; the mass ratio of the nano tourmaline powder to the graphene oxide is 1:1, and the addition amounts of the carbon disulfide, the urea and the epoxy hexane are all 1% of the mass of the bamboo fiber.
S2: adding nano tourmaline powder into an ethanol water solution, performing ultrasonic dispersion, then adding gamma-methacryloxypropyl trimethoxy silane and beta-cyclodextrin, uniformly stirring, then adding a starch water solution, and performing ultrasonic dispersion to obtain a mixture B; placing the fiber yarn prepared in the step S2 into the mixture B, standing and soaking for 18 hours at the temperature of 2 ℃, and carrying out low-temperature vacuum drying to obtain modified fiber yarn; wherein, the mass ratio of the nano tourmaline powder to the double bond silane coupling agent to the beta-cyclodextrin is 1:0.1:1.5; the mass ratio of the nano tourmaline powder to the starch is 1:3, a step of;
s3: taking the modified fiber yarn prepared in the step S2 as a core material, and cotton fiber as an outer fiber layer, and spinning to obtain core spun yarns;
s4: soaking the core spun yarn in water for 3 times for 20min each time, and naturally airing.
Example 2
S1, crushing bamboo fibers to 1-2cm, soaking the bamboo fibers in a sodium hydroxide solution with the mass fraction of 4% for 30min, heating the system to 45 ℃, adding carbon disulfide liquid into a reaction system at the temperature, uniformly stirring, preserving the heat for 6h, and introducing nitrogen into the reaction system through an aeration device in the heat preservation process to obtain a cellulose solution; mixing nano tourmaline powder with graphene oxide aqueous solution, and performing ultrasonic dispersion to obtain a mixture A; adding urea into the cellulose solution, uniformly stirring, adding epichlorohydrin, and stirring for 1.5h; adding the mixture A and the water-soluble polyethylene glycol solution at the same time, and stirring for 2 hours to obtain spinning solution; filtering and defoamating the spinning solution, and adding the filtered and defoamed spinning solution into a spinning bath with the temperature of 45 ℃ for spinning and forming to obtain fiber yarns; wherein the spinning bath comprises: 80g/L of sulfuric acid, 150g/L of sodium sulfate and 5g/L of zinc sulfate; the mass ratio of the nano tourmaline powder to the water-soluble polyethylene glycol is 1:1, a step of; the mass ratio of the nano tourmaline powder to the graphene oxide is 1:1, and the addition amounts of the carbon disulfide, the urea and the epoxy hexane are all 1% of the mass of the bamboo fiber.
S2: adding nano tourmaline powder into an ethanol water solution, performing ultrasonic dispersion, then adding gamma-methacryloxypropyl trimethoxy silane and beta-cyclodextrin, uniformly stirring, then adding a starch water solution, and performing ultrasonic dispersion to obtain a mixture B; placing the fiber yarn prepared in the step S2 into the mixture B, standing and soaking for 18 hours at the temperature of 2 ℃, and carrying out low-temperature vacuum drying to obtain modified fiber yarn; wherein, the mass ratio of the nano tourmaline powder to the double bond silane coupling agent to the beta-cyclodextrin is 1:0.2:2; the mass ratio of the nano tourmaline powder to the starch is 1:3, a step of;
s3: taking the modified fiber yarn prepared in the step S2 as a core material, and cotton fiber as an outer fiber layer, and spinning to obtain core spun yarns;
s4: soaking the core spun yarn in water for 3 times for 20min each time, and naturally airing.
Example 3
S1, crushing bamboo fibers to 1-2cm, soaking the bamboo fibers in a sodium hydroxide solution with the mass fraction of 2% for 30min, heating the system to 55 ℃, adding carbon disulfide liquid into a reaction system at the temperature, uniformly stirring, preserving the heat for 5h, and introducing nitrogen into the reaction system through an aeration device in the heat preservation process to obtain a cellulose solution; mixing nano tourmaline powder with graphene oxide aqueous solution, and performing ultrasonic dispersion to obtain a mixture A; adding urea into the cellulose solution, uniformly stirring, adding epichlorohydrin, and stirring for 2 hours; adding the mixture A and the water-soluble polyethylene glycol solution at the same time, and stirring for 2 hours to obtain spinning solution; filtering and defoamating the spinning solution, and adding the filtered and defoamed spinning solution into a spinning bath with the temperature of 40 ℃ for spinning and forming to obtain fiber yarns; wherein the spinning bath comprises: 80g/L of sulfuric acid, 150g/L of sodium sulfate and 5g/L of zinc sulfate; the mass ratio of the nano tourmaline powder to the water-soluble polyethylene glycol is 1:0.8; the mass ratio of the nano tourmaline powder to the graphene oxide is 1:1.5, and the addition amounts of the carbon disulfide, the urea and the epoxy hexane are all 1% of the mass of the bamboo fiber.
S2: adding nano tourmaline powder into an ethanol water solution, performing ultrasonic dispersion, then adding gamma-methacryloxypropyl trimethoxy silane and beta-cyclodextrin, uniformly stirring, then adding a starch water solution, and performing ultrasonic dispersion to obtain a mixture B; placing the fiber yarn prepared in the step S2 into the mixture B, standing and soaking for 18 hours at the temperature of 1 ℃, and carrying out low-temperature vacuum drying to obtain modified fiber yarn; wherein, the mass ratio of the nano tourmaline powder to the double bond silane coupling agent to the beta-cyclodextrin is 1:0.5:1.5; the mass ratio of the nano tourmaline powder to the starch is 1:3, a step of;
s3: taking the modified fiber yarn prepared in the step S2 as a core material, taking ramie fiber as an outer fiber layer, and spinning to obtain core spun yarn;
s4: soaking the core spun yarn in water for 3 times for 20min each time, and naturally airing.
Example 4
S1, crushing bamboo fibers to 1-2cm, soaking the bamboo fibers in a sodium hydroxide solution with the mass fraction of 2% for 30min, heating the system to 55 ℃, adding carbon disulfide liquid into a reaction system at the temperature, uniformly stirring, preserving the heat for 6h, and introducing nitrogen into the reaction system through an aeration device in the heat preservation process to obtain a cellulose solution; mixing nano tourmaline powder with graphene oxide aqueous solution, and performing ultrasonic dispersion to obtain a mixture A; adding urea into the cellulose solution, uniformly stirring, adding epichlorohydrin, and stirring for 2 hours; adding the mixture A and the water-soluble polyethylene glycol solution at the same time, and stirring for 2 hours to obtain spinning solution; filtering and defoamating the spinning solution, and adding the filtered and defoamed spinning solution into a spinning bath with the temperature of 40 ℃ for spinning and forming to obtain fiber yarns; wherein the spinning bath comprises: 80g/L of sulfuric acid, 150g/L of sodium sulfate and 5g/L of zinc sulfate; the mass ratio of the nano tourmaline powder to the water-soluble polyethylene glycol is 1:0.5; the mass ratio of the nano tourmaline powder to the graphene oxide is 1:1, and the addition amounts of the carbon disulfide, the urea and the epoxy hexane are all 1% of the mass of the bamboo fiber.
S2: adding nano tourmaline powder into an ethanol water solution, performing ultrasonic dispersion, then adding gamma-methacryloxypropyl trimethoxy silane and beta-cyclodextrin, uniformly stirring, then adding a starch water solution, and performing ultrasonic dispersion to obtain a mixture B; in the mixture B, an antibacterial agent is added, and the antibacterial agent comprises the following raw materials in parts by weight: placing 10 parts of chitosan quaternary ammonium salt, 5 parts of titanium dioxide and 1 part of potassium persulfate in a mixture B added with an antibacterial agent, stirring for 4 hours at 60 ℃, then cooling to 2 ℃, standing and soaking for 18 hours at the temperature, and drying in vacuum at low temperature to obtain modified fiber; wherein, the mass ratio of the nano tourmaline powder to the double bond silane coupling agent to the beta-cyclodextrin is 1:0.1:1.5; the mass ratio of the nano tourmaline powder to the starch is 1:3, the addition mass of the antibacterial agent is 5% of the dry weight mass of the fiber;
s3: taking the modified fiber yarn prepared in the step S2 as a core material, taking bamboo fiber as an outer fiber layer, and spinning to obtain core spun yarns;
s4: soaking the core spun yarn in water for 3 times for 20min each time, and naturally airing.
Example 5
The difference from example 1 is that in this example, the mass ratio of the nano tourmaline powder, the double bond silane coupling agent and the beta-cyclodextrin is 1:0.5:3, a step of; the remainder was the same as in example 1.
Example 6
The difference from example 1 is that in this example, the mass ratio of the nano tourmaline powder, the double bond silane coupling agent and the beta-cyclodextrin is 1:0.1:3, a step of; the remainder was the same as in example 1.
Example 7
The difference from example 1 is that in this example, the mass ratio of nano tourmaline powder to starch is 1:2; the remainder was the same as in example 1.
Example 8
The difference from example 1 is that in this example, the mass ratio of nano tourmaline powder to starch is 1:5, a step of; the remainder was the same as in example 1.
Example 9
The difference from example 1 is that in this example, the silane coupling agent is vinyltriethoxysilane; the remainder was the same as in example 1.
Example 10
The difference from example 1 is that in this example, the silane coupling agent is vinyltrimethoxysilane; the remainder was the same as in example 1.
Example 11
The difference from example 4 is that in this example, the antibacterial agent comprises the following raw materials in parts by weight: 20 parts of chitosan quaternary ammonium salt, 10 parts of titanium dioxide and 1 part of potassium persulfate; the remainder was the same as in example 4.
Example 12
The difference from example 4 is that in this example, the antibacterial agent comprises the following raw materials in parts by weight: 15 parts of chitosan quaternary ammonium salt, 5 parts of titanium dioxide and 0.5 part of potassium persulfate; the remainder was the same as in example 4.
Comparative example 1
The difference from example 1 is that in step S2 in this comparative example, the silane coupling agent and β -cyclodextrin are not added, and the rest is the same as example 1.
Comparative example 2
The difference from example 1 is that in step S2 in this comparative example, the same amount of water was directly added without adding the starch aqueous solution, and the rest was the same as in example 1.
Comparative example 3
The difference from example 4 is that in step S2 in this comparative example, the silane coupling agent and starch are not added, and the remainder is the same as example 4.
Experimental example
The fibers of examples 1 to 12 and comparative examples 1 to 3 were woven into layers of cloth by a weaving process, and a plurality of pieces of cloth having the same size were cut out for use.
1. Determination of fabric anion occurrence
The negative ion generation amounts before washing, after washing 1 time, after washing 10 times, after washing 20 times and after washing 50 times were tested by using GB/T30128-2013 detection and evaluation of negative ion generation amount of textiles, respectively, and the results are shown in Table 1. The washing step is to put the cloth in deionized water, soak for 10min, knead for 10 times, soak for 10min again, and then take out and dry naturally. Wherein, the value of each item in Table 1 is an average value of the generation amount of 3 cloth negative ions.
TABLE 1 anion generating capacity of fabrics (in units of cm) 3 )
Before water washing Washing with water for 1 time Washing with water for 10 times After washing 20 times Washing with water for 50 times
Example 1 1584 1526 1423 1221 985
Example 2 1523 1501 1452 1214 1015
Example 3 1563 1522 1421 1189 987
Example 4 1549 1509 1411 1175 1011
Example 5 1535 1489 1421 1201 992
Example 6 1426 1403 1345 1153 1001
Example 7 1526 1488 1406 1179 897
Example 8 1589 1511 1475 1203 1021
Example 9 1475 1423 1369 1147 951
Example 10 1533 1478 1401 1158 963
Example 11 1584 1514 1475 1143 976
Example 12 1563 1508 1426 1154 984
Comparative example 1 1024 874 654 312 112
Comparative example 2 1102 1011 845 640 401
Comparative example 3 1032 984 723 511 321
As can be seen from the data in table 1, the fabrics of examples 1 to 12 have reduced negative ion generation with increased number of water washing, because tourmaline is inevitably fallen off in a small amount during the water washing and kneading process, and the corresponding negative ion generation is reduced after the number of tourmaline is reduced. However, the fabrics of examples 1-12 still had a higher occurrence after 20 washes and a higher occurrence after 50 washes. However, the cloth of comparative examples 1 to 3 showed a remarkable decrease in the amount of negative ions generated after washing with water 50, indicating that tourmaline was largely removed during the washing process. The reason for this is that in comparative example 1, the tourmaline added in step S2 cannot be wrapped without adding the coupling agent and cyclodextrin, and has low bonding strength with the inner layer fiber, and after a plurality of water washes, the tourmaline of this part is largely fallen off, thereby causing a rapid decrease in the amount of negative ions generated. In comparative example 2, which does not add starch, i.e., the gap between the inner fiber and the outer fiber is small, tourmaline falls off more than in the comparative example, and the negative ion generation amount is correspondingly reduced.
2. Antibacterial test
Antibacterial properties were tested with reference to GB/T20944.3-2008, specifically using E.coli (ATCC 25922), measured in terms of antibacterial rate. The antibacterial ratio was an average value of 3 cloths, and the results are shown in table 2.
TABLE 2 antibacterial Rate (%)
Before water washing Washing with water for 1 time Washing with water for 10 times After washing 20 times Washing with water for 50 times
Example 4 98.2 97.6 95.4 92.3 90.2
Example 11 97.3 95.8 94.3 91.1 89.5
Example 12 97.5 95.3 91.2 89.1 88.5
Comparative example 3 96.3 90.2 75.3 54.1 36.2
As can be seen from table 2, the cloths of examples 4, 11 and 12, which have excellent antibacterial properties, were able to reach about 90% in antibacterial property after washing with water several times, but for comparative example 3, a silane coupling agent was not added in the process of preparing the fiber yarn, so that the binding fastness of chitosan quaternary ammonium salt to the fiber was low, and after washing with water several times, the antibacterial agent was peeled off, resulting in a decrease in antibacterial effect.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the invention is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

Claims (10)

1. The preparation process of the negative oxygen ion air purification material is characterized by comprising the following steps of:
s1: mixing nano tourmaline powder with graphene oxide aqueous solution, and performing ultrasonic dispersion to obtain a mixture A; adding urea into the cellulose solution, uniformly stirring, adding epichlorohydrin, and stirring for 1-2h; adding the mixture A and the water-soluble polyethylene glycol solution at the same time, and stirring for 1-2h to obtain spinning solution; spinning and forming the spinning solution to obtain fiber yarns;
s2: adding nano tourmaline powder into an ethanol water solution, performing ultrasonic dispersion, adding a double bond silane coupling agent and beta-cyclodextrin, uniformly stirring, adding a starch water solution, and performing ultrasonic dispersion to obtain a mixture B; placing the fiber yarn prepared in the step S2 into the mixture B, standing for 15-18h at 1-2 ℃, and carrying out low-temperature vacuum drying to obtain modified fiber yarn;
s3: taking the modified fiber yarn prepared in the step S2 as a core material, taking plant fiber as an outer fiber layer, and spinning to obtain core spun yarn;
s4: soaking the core spun yarn in water for multiple times, and naturally airing.
2. The process for preparing a negative oxygen ion air purification material according to claim 1, wherein the cellulose solution is prepared by the steps of: pulverizing bamboo fiber, soaking in sodium hydroxide solution, heating to 45-55deg.C, adding carbon disulfide into the reaction system at the temperature, stirring, and maintaining the temperature for 5-6 hr to obtain cellulose solution.
3. The process for preparing a negative oxygen ion air purification material according to claim 2, further comprising: in the heat preservation process, inert gas is introduced into the reaction system through an aeration device.
4. The process for preparing a negative oxygen ion air purification material according to claim 1, wherein the double bond silane coupling agent is gamma-methacryloxypropyl trimethoxysilane, vinyl triethoxysilane or vinyl trimethoxysilane.
5. The process for preparing a negative oxygen ion air-purifying material according to claim 1, wherein in the step S2, an antibacterial agent is added to the mixture B;
wherein the antibacterial agent comprises the following raw materials in parts by weight: 10-20 parts of chitosan quaternary ammonium salt, 5-10 parts of titanium dioxide and 0.5-1 part of potassium persulfate.
6. The process for preparing a negative oxygen ion air purification material according to claim 1, wherein the plant fiber is one or more of cotton fiber, bamboo fiber, ramie fiber and sisal fiber.
7. The method for preparing a negative oxygen ion air purification material according to claim 1, wherein in the step S2, the mass ratio of the nano tourmaline powder, the double bond silane coupling agent and the beta-cyclodextrin is 1: (0.1-0.5): (1.5-3).
8. The method for preparing a negative oxygen ion air purification material according to claim 1, wherein in the step S1, a mass ratio of the nano tourmaline powder to the water-soluble polyethylene glycol is 1: (0.5-1).
9. The method for preparing a negative oxygen ion air-purifying material according to claim 6, wherein in the step S2, a mass ratio of nano tourmaline powder to starch is 1: (2-5).
10. A negative oxygen ion air purification material, characterized by being prepared by the preparation process of any one of claims 1-9.
CN202311553914.6A 2023-11-21 2023-11-21 Negative oxygen ion air purification material and preparation process thereof Pending CN117547922A (en)

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