WO2020233125A1 - 用于织物功能整理的大气压等离子体设备及其应用 - Google Patents

用于织物功能整理的大气压等离子体设备及其应用 Download PDF

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Publication number
WO2020233125A1
WO2020233125A1 PCT/CN2019/129709 CN2019129709W WO2020233125A1 WO 2020233125 A1 WO2020233125 A1 WO 2020233125A1 CN 2019129709 W CN2019129709 W CN 2019129709W WO 2020233125 A1 WO2020233125 A1 WO 2020233125A1
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Prior art keywords
pipeline
grafting
gas
electrode
plasma generator
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PCT/CN2019/129709
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English (en)
French (fr)
Inventor
周嫦娥
王红卫
沈文凯
范蕾
巨鑫
张国政
杨童心
王婉宁
孙昌
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江南大学
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Publication of WO2020233125A1 publication Critical patent/WO2020233125A1/zh
Priority to US17/215,261 priority Critical patent/US11946196B2/en

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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00—Generating plasma; Handling plasma
    • H05H1/24—Generating plasma
    • H05H1/48—Generating plasma using an arc
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/08—Organic compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating 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
    • D06M11/07—Treating 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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating 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
    • D06M11/07—Treating 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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/30—Treating 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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with oxides of halogens, oxyacids of halogens or their salts, e.g. with perchlorates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
    • D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
    • D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
    • D06M14/20—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of natural origin
    • D06M14/22—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of natural origin of vegetal origin, e.g. cellulose or derivatives thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00—Generating plasma; Handling plasma
    • H05H1/24—Generating plasma
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10—Repellency against liquids
    • D06M2200/11—Oleophobic properties
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10—Repellency against liquids
    • D06M2200/12—Hydrophobic properties
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30—Flame or heat resistance, fire retardancy properties
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H2245/00—Applications of plasma devices
    • H05H2245/40—Surface treatments

Definitions

  • the invention relates to an atmospheric pressure plasma equipment for the functional finishing of fabrics and its application, and belongs to the field of textile printing and dyeing engineering.
  • the textile industry is a traditional pillar industry in my country, including textile, dyeing and finishing, clothing and textile special equipment manufacturing.
  • my country's printing and dyeing industry has entered a period of rapid development.
  • the equipment and technical level have been significantly improved, and the production technology and equipment have been continuously updated.
  • Dyeing and finishing has occupied a pivotal position in the textile industry. Cost control in the dyeing and finishing process directly affects the economic value of the fabric. Therefore, the cost of finishing the fabric must be strictly controlled.
  • the pre-treatment and post-finishing methods of fabrics are wet treatment, which produces a large amount of waste water containing complex chemical substances, which not only causes waste of resources, but also causes environmental pollution. Therefore, there is an urgent need for a processing method with little or no water in the dyeing and finishing industry.
  • the small liquor ratio dyeing equipment, short-flow dyeing process, digital inkjet printing technology, sublimation transfer printing technology, foam finishing system and waste heat recovery technology have alleviated the pollution of the dyeing and finishing industry to a certain extent, the existing clean
  • the production technology still has problems such as wastewater pollution and high energy consumption.
  • supercritical carbon dioxide printing and dyeing technology and vacuum plasma technology can achieve waterless dyeing and finishing, there are still technical problems in industrial production due to high pressure and vacuum conditions, respectively.
  • the atmospheric plasma equipment is applied in the textile printing and dyeing industry
  • the present invention provides an atmospheric pressure plasma equipment that can continuously finish fabrics and its application.
  • the atmospheric pressure plasma equipment of the present invention can realize continuous post-finishing processing of textiles under atmospheric pressure conditions and solve traditional printing and dyeing processing. Problems of medium to high sewage and high energy consumption.
  • the present invention first provides an atmospheric pressure plasma equipment.
  • the atmospheric pressure plasma equipment includes a carrier gas pipeline 1, a reactive gas pipeline 2, a carrier gas pipeline 6, a graft gas pipeline 14, a second A pipeline 15, a second pipeline 16, a third pipeline 17, a single electrode plasma generator negative 24 and a single electrode plasma generator positive 25, wherein the third pipeline 17 is connected to the single electrode plasma generator
  • the negative electrode 24 is connected to the single-electrode plasma generator composed of the positive electrode 25 of the single-electrode plasma generator
  • the gas in the third pipe 17 is a combination of the gas in the first pipe 15 or the gas in the second pipe 16, and
  • the gas of the first pipeline 15 is formed by the combination of the carrier gas of the carrier gas pipeline 1 and the reaction gas of the reactive gas pipeline 2, and the gas of the second pipeline 16 is composed of the carrier gas of the carrier gas pipeline 6.
  • the grafting gas of the grafting gas pipeline 14 is obtained from the grafted monomers vaporized in the grafting tank 8; the carrier gas pipeline 1, the reactive gas pipeline 2, the carrier gas pipeline 6 and the grafting gas A solenoid valve 4 and a flow meter 5 are installed on the pipeline 14;
  • the single-electrode plasma generator composed of the single-electrode plasma generator negative electrode 24 and the single-electrode plasma generator positive electrode 25 is connected to the power matching device 26 through a power cord, and the single-electrode plasma generator is located in the housing 29 Inside, the power supply matching device 26, the cloth guide roller 2 and the cloth guide roller 21 with a speed regulating motor are respectively located outside the cover 29, and the cloth guide roller 28 and the cloth guide roller 21 with a speed regulating motor are respectively arranged on the cover
  • the two sides of the shell 29 are parallel to each other, and the shell 29 has holes for the fabric and the power cord to enter and exit.
  • the single electrode plasma generator negative electrode 24 is two rectangular parallelepiped aluminum alloy blocks, and the single electrode plasma generator positive electrode 25 is an aluminum alloy tube sheathed with a glass tube;
  • the negative pole 24 of the generator and the positive pole 25 of the single-electrode plasma generator are fixed by metal screws, tetrafluoroethylene insulating blocks at both ends of the electrodes and an aluminum alloy jacket to form a single-electrode plasma generator.
  • the single-electrode plasma generator includes a condensing device
  • the condensing device includes a condensed water inlet pipe (19), a condensate pipe, and a condensed water outlet pipe (20), and the three are sequentially Connected, the cold water inlet pipe (19) and cold water outlet pipe (20) are respectively located at two ends of the electrode plasma generator, and the condensing pipe passes through the electrode plasma generator to prevent the electrode from overheating.
  • the grafted gas pipeline 14, the solenoid valve 4 and the flow meter 5 on the grafted gas pipeline 14, the second pipeline 16 and the third pipeline 17 are all equipped with thermal insulation Layer to prevent condensation of the grafting monomer gas.
  • a copper tube is placed in the negative electrode 24 of the single-electrode plasma generator.
  • the copper tube is provided with small holes as the gas outlet 18, and the gas outlet 18 is located in the single-electrode plasma generator.
  • the gas in the third pipeline 17 enters the single-electrode plasma generator through the gas outlet 18 on the negative electrode of the single-electrode plasma generator.
  • the power matching device 26 is connected to a power source through a power cord, and the power source is located outside the casing 29.
  • the heating device 10 is used to heat the grafted monomer to vaporize it, and enter the single electrode through the grafted gas pipeline 14, the second pipeline 16, and the third pipeline 17.
  • Plasma generator the heating device 10 is connected to a temperature control heating module 12, the temperature control heating module 12 includes a heating power supply and a temperature control device for providing heat and controlling the heating temperature.
  • the grafting tank 8 is provided with a liquid adding port 13 for adding the grafting monomer to the grafting tank 8.
  • a liquid level measuring rod 9 is installed at the filling port 13 of the grafting tank 8, and the liquid level measuring rod 9 is used to measure the liquid level of the grafting liquid 11.
  • the material of the cover 29 is preferably organic glass.
  • the fabric is parallel to the single-electrode plasma generator, and when the fabric 27 is placed on the cloth guide roller and passes under the single-electrode plasma generator, the atmospheric plasma interaction is achieved. Continuous processing of fabrics.
  • the casing 29 has an exhaust port 23 and a fan 22 connected to the exhaust port 23 for collecting the remaining unreacted gas.
  • the discharge electrode is placed in the glass cover to facilitate collection of exhaust gas and uniform discharge.
  • the type of gas or graft monomer used in the instrument corresponds to the effect of fabric treatment. Different fabric finishing effects require different gases or graft monomers.
  • the carrier gas when it is antibacterial finishing, is helium or argon; the reaction gas is ammonia or nitrogen, or the grafting monomer is a nitrogen-containing small molecule Organic monomers, wherein the nitrogen-containing small molecule organic monomers include methylamine, ethylenediamine, 1,2-propanediamine, propargylamine, isopropylamine, diisopropylamine, n-propylamine, di-n-propylamine, etc. Of any kind.
  • the carrier gas when it is water and oil repellent finishing, is helium or argon; the reaction gas is carbon tetrafluoride, or the grafting monomer is difluoro Ethylene, tetrafluoroethylene, hexafluoroethylene, etc.
  • the carrier gas is helium or argon;
  • the reaction gas is a mixed gas of carbon tetrafluoride and methane, or the graft monomer For acrylic.
  • the carrier gas when it is antistatic finishing, is helium or argon; the reaction gas is sulfur dioxide, or the grafting monomer is acrylic acid, vinyl monomer, etc. .
  • the flow rate of the gas can be controlled by a flow meter to achieve stable plasma release.
  • the carrier gas needs to carry the grafted monomer into the discharge device to ensure stable discharge and plasma output.
  • the cloth guide roller with a speed-adjustable motor includes a speed switch for controlling the speed of fabric transport.
  • the present invention also provides a method for functionally finishing fabrics by the atmospheric pressure plasma grafting method, which is performed on an atmospheric pressure plasma equipment.
  • the steps of the method are
  • the carrier gas of the carrier gas pipeline (1) and the reactive gas of the reactive gas pipeline (2) are in the first pipeline (15). ), enter the third pipeline (17), enter the single-electrode plasma generator through the air outlet (18) on the negative electrode of the single-electrode plasma generator for plasmaization;
  • the grafting monomer is added to the grafting tank (8), and the grafting monomer is heated by the heating device to vaporize the grafting monomer, and then the grafting gas pipeline (14), and merge with the gas in the carrier gas pipeline (6) in the second pipeline (16), enter the third pipeline (17), and pass through the gas outlet (18) on the negative electrode of the single-electrode plasma generator Enter the single-electrode plasma generator for plasmaization;
  • the functional finishing includes antibacterial finishing, water and oil repellent finishing, flame retardant finishing, antistatic finishing and the like.
  • the carrier gas when it is antibacterial finishing, is helium or argon; the reaction gas is ammonia and or nitrogen; the grafting monomer is a small nitrogen-containing molecule Organic monomers, wherein the nitrogen-containing small molecule organic monomers include methylamine, ethylenediamine, 1,2-propanediamine, propargylamine, isopropylamine, diisopropylamine, n-propylamine, di-n-propylamine, and the like.
  • the carrier gas when it is water and oil repellent finishing, is helium or argon; the reaction gas is carbon tetrafluoride; the grafting monomer is ethylene difluoride , Tetrafluoroethylene, hexafluoroethylene and other fluorocarbon compounds.
  • the carrier gas when it is flame retardant finishing, is helium or argon; the reaction gas is carbon tetrafluoride, or the grafting monomer is acrylic acid.
  • the carrier gas when it is antistatic finishing, is helium or argon; the reaction gas is sulfur dioxide, or the grafting monomer is acrylic acid, vinyl monomer, etc. .
  • the flow rates of the carrier, the reaction gas, and the graft monomer need to be adjusted according to the finishing effect and the conditions of plasmaization of the reaction gas and the monomer gas, respectively.
  • the heating temperature of the heating cup is based on the ability of the grafted monomer to vaporize.
  • the plasma-ized monomers are rearranged and polymerized on the surface of the fabric 27, and nitrogen-containing groups are introduced on the surface of the fabric. After chlorination with sodium hypochlorite solution, the fabric is given antibacterial effect.
  • the operating parameters of plasmaization are: carrier gas flow rate is 1-15L/min, monomer vaporization temperature is 0-200°C, holding temperature is 0-200°C, and flow rate is 0.006 -0.06L/min, power supply is 0-500W.
  • the speed of the fabric conveying is controlled by a motor on the cloth guide roller, and the speed range is 0.001-0.1 m/s.
  • the equipment changes the existing plasma intermittent processing method to realize continuous plasma processing of the fabric.
  • the equipment and method of the present invention realize the functional finishing of fabrics under anhydrous conditions.
  • This treatment process has rapid response, short time-consuming, high efficiency, environmental protection, simple operation, uniform treatment effect, and no effect on fabrics. Selectivity and does not change the nature of the fabric itself.
  • Figure 1 is a schematic diagram of the structure of the plasma machine of the present invention; among them, 1. carrier gas pipeline, 2. reactive gas pipeline, 3. control cabinet, 4. solenoid valve, 5. flowmeter, 6. carrier gas pipe Road, 7, grafting instrument, 8, grafting tank, 9, liquid level measuring stick, 10, heating equipment, 11, grafting liquid, 12, temperature control heating module, 13, filling port, 14, grafting gas Pipeline, 15, the first pipeline, 16, the second pipeline, 17, the third pipeline, 18, the air outlet, 19, the condensate water inlet pipe, 20, the condensate water outlet pipe, 21, with a speed regulating motor
  • Plexiglass cover The cloth guide roller, 22, fan, 23, air outlet, 24, single electrode plasma generator negative pole, 25, single electrode plasma generator positive pole, 26, power matching device, 27, fabric, 28, cloth guide roller , 29. Plexiglass cover.
  • FIG. 2 Schematic diagram of the structure of a single-electrode plasma generator.
  • Figure 3 XPS spectra of elements on the surface of cotton fabric before and after plasma grafting.
  • Figure 4 (a) before plasma deposition treatment (b) after plasma deposition treatment (c) after plasma deposition treatment and chlorinated cotton fabric SEM pictures.
  • Fig. 6 The influence of plasma (a) treatment time and (b) power on the tearing strength of the fabric.
  • the atmospheric pressure plasma equipment includes a carrier gas pipeline 1, a reactive gas pipeline 2, a carrier gas pipeline 6, a graft gas pipeline 14, a first pipeline 15, and a second
  • the pipeline 16 the third pipeline 17, the single electrode plasma generator negative electrode 24 and the single electrode plasma generator positive electrode 25, wherein the third pipeline 17 is connected to the single electrode plasma generator negative electrode 24 and the single electrode plasma generator
  • the single-electrode plasma generator composed of the generator positive electrode 25 is connected.
  • the gas of the third pipeline 17 is the gas of the first pipeline 15 or the gas of the second pipeline 16 is combined.
  • the first pipeline 15 The gas is composed of the carrier gas of the carrier gas pipeline 1 and the reaction gas of the reactive gas pipeline 2, and the gas of the second pipeline 16 is composed of the carrier gas of the carrier gas pipeline 6 and the graft gas pipeline 14
  • the grafting gas is combined; the other end of the grafting gas pipeline 14 is connected to the grafting tank 8.
  • a heating device 10 is installed on the outside of the grafting tank 8, and the heating device 10 is connected to the temperature control heating module 12
  • the temperature control heating module 12 includes a heating power supply and a temperature control device, a liquid level measuring rod 9 is provided at the filling port 13 of the grafting tank 8, and the grafting gas of the grafting gas pipeline 14 is a grafting tank 8 is obtained from the grafted monomer after vaporization;
  • the carrier gas pipeline 1, the reactive gas pipeline 2, the carrier gas pipeline 6 and the graft gas pipeline 14 are all equipped with a solenoid valve 4 and a flow meter 5;
  • the single-electrode plasma generator composed of the single-electrode plasma generator negative 24 and the single-electrode plasma generator positive 25 is connected to the power matching device 26 through a power cord, and the single-electrode plasma generator is located in the cover Inside the housing 29, the power supply, the power supply matching device 26, the cloth guide roller 2 and the cloth guide roller 21 with a speed regulating motor are respectively located outside
  • the casing 29 has holes for fabrics and power cords to enter and exit.
  • the casing 29 has an exhaust port 23 and a fan 22 connected to the exhaust port 23 for Collection of remaining gas; the fabric is parallel to the single-electrode plasma generator, when the fabric 27 is placed on the cloth guide roller and passes under the single-electrode plasma generator, continuous treatment of the fabric by atmospheric plasma is realized.
  • the negative electrode 24 of the single-electrode plasma generator is two rectangular aluminum alloy blocks
  • the positive electrode 25 of the single-electrode plasma generator is an aluminum alloy tube covered with a glass tube
  • the negative electrode 24 of the single-electrode plasma generator and the single-electrode plasma The positive pole 25 of the body generator is fixed by metal screws, the tetrafluoroethylene insulation block at both ends of the electrode and the aluminum alloy jacket to form a single-electrode plasma generator.
  • a copper tube is placed in the negative pole 24 of the single-electrode plasma generator.
  • a small hole is opened as a gas outlet 18, the outlet 18 is located above the positive electrode 25 of the single-electrode plasma generator; the single-electrode plasma generator includes a condensing device, and the condensing device includes a condensed water inlet pipe (19).
  • the condenser tube and the condensed water outlet pipe (20) are connected end to end.
  • the cold water inlet pipe (19) and the cold water outlet pipe (20) are respectively located at both ends of the electrode plasma generator.
  • the tube passes through the electrode plasma generator to prevent the electrode from overheating.
  • the grafted gas pipeline 14, the solenoid valve (4) and the flow meter (5) on the grafted gas pipeline (14), and the third pipeline 17 are all equipped with an insulating layer to prevent grafting The monomer gas condenses.
  • the heating device 10 is used to heat the grafted monomer to vaporize it, enter the grafting gas pipeline 14, merge with the carrier gas in the carrier gas pipeline 6 in the second pipeline 16, and enter the third pipeline.
  • the pipeline 17 enters the single-electrode plasma generator composed of the single-electrode plasma generator negative electrode 24 and the single-electrode plasma generator positive electrode 25 through the air outlet 18 on the negative electrode of the single-electrode plasma generator.
  • the fabric 27 is processed.
  • the material of the cover 29 is preferably organic glass.
  • the grafting liquid 11 is added to the grafting tank 8, and the heating power and temperature control device of the temperature control heating module 12 are turned on to provide heat and control the heating temperature so that the grafting liquid Heating gasification.
  • the vaporized graft monomer enters the graft gas pipeline 14, merges with the carrier gas in the carrier gas pipeline 6 in the second pipeline 16, and enters the third pipeline 17.
  • the fabric 27 is placed on the cloth guide roller and passes under the single-electrode plasma generator, continuous treatment of the fabric by atmospheric plasma is realized.
  • the continuous treatment of the fabric by atmospheric plasma is realized, the dry finishing of the fabric is realized, and no waste water is generated, so as to realize the cleaning and finishing of the fabric.
  • the plasma-ized monomers are rearranged and polymerized on the surface of the fabric 27, nitrogen-containing groups are introduced on the surface of the fabric, and chlorinated with a 1.0 wt% sodium hypochlorite solution to give the fabric an antibacterial effect.
  • the XPS element analysis spectrum of the fabric surface after plasma treatment with nitrogen-containing small molecule organic monomers is shown in Figure 3. It can be seen from Figure 3 that after the plasma grafting method treats the cotton fabric, the surface of the cotton fabric contains nitrogen. In other words, after plasma treatment of the fabric with nitrogen-containing small molecule organic monomers, nitrogen can be introduced on the surface of the fabric. According to the XPS test results, the calculation of the element content on the surface of the fabric is shown in Table 1. It can be seen from Table 1 that before the plasma deposition treatment of cotton fabric, the surface of the fabric is composed of C and O elements, the content of which is 72.46% and 27.54%, respectively.
  • the element composition on the surface of the cotton fabric is C and O
  • the contents of N and N are 68.70%, 17.28%, and 14.02%, respectively. Therefore, the nitrogen-containing small molecule organic monomer plasma is deposited on the surface of the cotton fabric, thereby reducing the content of C and O elements.
  • the SEM image of the fabric surface after plasma treatment with nitrogen-containing small molecule organic monomers is shown in Figure 4. It can be seen from Figure 4 that compared with the cotton fabric without plasma treatment, after plasma treatment, there are many pits and net-like structures on the surface of cotton fiber, and even after sodium hypochlorite chlorination, these pits and nets The shape structure still exists. It can be seen from the SEM image that the nitrogen-containing small molecule organic monomer plasma treatment of the cotton fabric will damage the cotton fiber, but the damage is not significant. The damage degree of the fabric after plasma treatment was tested by the grating method, as shown in Figure 5. The grating method test in Fig. 5 further confirms that compared with untreated cotton fabric, the damage size of the plasma to the fiber is 300-450nm. Therefore, the damage to the fabric treated by nitrogen-containing small molecule organic monomer plasma is not obvious.
  • Figure 6 is a test result of the effect of treatment time and power on the tearing strength of the fabric in plasma treatment. It can be seen from the figure that the treatment time is less than 4min and the power is less than 1400w. Compared with the fabric without plasma treatment, the tearing strength of the fabric after plasma treatment is increased, indicating that plasma deposition can be enhanced The tearing strength of the fabric can compensate for the strength loss of the fabric caused by plasma etching.
  • Gas, the flow rate is 6L/min) merge in the first pipeline 15, enter the third pipeline 17, and enter the negative electrode 24 and the single electrode through the gas outlet 18 on the negative electrode of the single electrode plasma generator.
  • the single-electrode plasma generator composed of the positive electrode 25 of the plasma generator, the power is 300W, and it is plasmaized;
  • the plasmaized monomers are rearranged and polymerized on the surface of the fabric 27, and fluorine is introduced on the surface of the fabric.
  • Measuring the contact angle of the fabric Use the OCA40 video contact angle measuring instrument to test the contact angle between the fabric and water. The amount of water is 5 ⁇ L, and the water droplet is in contact with the fabric for 60 seconds. Measure 4 times at different positions of the same sample and take the average value. Test the cotton fabric before washing and after washing 15 times. The contact angle before washing can reach 148.7°, and the contact angle after washing 15 times is 136.5°, achieving a good water repellent effect.
  • Plasma-ized monomers are rearranged and polymerized on the surface of the fabric 27.
  • the finished fabric is ignited by the vertical combustion method (GB/T20286-2006) for 12 seconds and the limiting oxygen index (LOI) is measured: 26.3%. 2s, damaged char length: 15.6mm; and untreated fabric limit oxygen index (LOI): 19.1%, afterburning time: 9s, damaged char length: 30.5mm.
  • LOI limiting oxygen index

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Plasma & Fusion (AREA)
  • Physics & Mathematics (AREA)
  • Biochemistry (AREA)
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Abstract

一种用于织物功能整理的大气压等离子体设备及其应用，属于纺织印染工程领域。所述大气压等离子体设备，包括放电装置、接枝仪和传动装置，可以在大气压条件下，对织物进行等离子体连续处理，包括等离子体刻蚀和等离子体接枝，突破了真空等离子体设备间歇式加工的弊端；设备和方法在无水的条件下，实现了织物的抗菌整理，这一处理过程反应迅速、耗时短、高效、环保、操作简单、处理效果均一、对织物的没有选择性以及不改变织物本身的性质。

Description

[根据细则37.2由ISA制定的发明名称]　用于织物功能整理的大气压等离子体设备及其应用 技术领域
本发明涉及一种用于织物功能整理的大气压等离子体设备及其应用，属于纺织印染工程领域。
背景技术
纺织工业是我国传统的支柱产业，包括纺织、染整、服装和纺织专用设备制造等。随着国民经济的快速发展，我国印染行业进入了高速发展期，设备和技术水平明显提升，生产工艺和设备不断更新，染整加工在纺织工业中占据着举足轻重的地位。染整工艺中的成本管控直接影响到织物的经济价值。因此，对织物的整理过程要严格的控制成本。
传统的工艺中，织物前处理和后整理方式都是湿处理，产生大量的含有复杂化学物质的废水，不仅造成资源浪费，还造成环境污染。因此，在染整加工行业中急需一种少水甚至无水的加工方式。虽然目前出现的小浴比染色设备、短流程染色工艺、数码喷墨印花技术、升华转移印花技术、泡沫整理系统以及余热回收技术对染整行业的污染起到一定的缓解作用，但现有清洁生产技术仍存在着废水污染、能耗高等问题。超临界二氧化碳印染技术和真空等离子体技术虽然可以实现无水染整加工，但分别因高压条件和真空条件在工业化生产上还存在技术难题。
发明内容
【技术问题】
现有染整技术还不能完全解决行业的高污染和高能耗问题。
【技术方案】
针对上述问题，在本发明中，大气等离子设备在纺织印染行业中应用，
本发明提供了一种可以对织物进行连续式整理的大气压等离子体设备及其应用，利用本发明的大气压等离子体设备，能够实现在大气压条件下，实现纺织品的连续后整理加工，解决传统印染加工中高污水和高能耗的问题。
具体的，本发明首先提供了一种大气压等离子体设备，所述的大气压等离子体设备包括载体气体管路1、反应性气体管路2、载体气体管路6、接枝气体管路14、第一管路15、第二管路16、第三管路17、单电极等离子体发生器负极24和单电极等离子体发生器正极25，其中，第三管路17与由单电极等离子体发生器负极24和单电极等离子体发生器正极25组成的单电极等离子体发生器相连，所述第三管路17的气体为第一管路15的气体或第二管路16 的气体汇合而成，所述第一管路15的气体由载体气体管路1的载体气体和反应性气体管路2的反应气体汇合而成，所述第二管路16的气体由载体气体管路6的载体气体和接枝气体管路14的接枝气体汇合而成；所述接枝气体管路14的另一端与接枝罐8相连，所述接枝罐8的外部安装有加热设备10，所述接枝气体管路14的接枝气体是接枝罐8内气化后的接枝单体得到的；所述载体气体管路1、反应性气体管路2、载体气体管路6和接枝气体管路14上均安装有电磁阀4和流量计5；
所述由单电极等离子体发生器负极24和单电极等离子体发生器正极25组成的单电极等离子体发生器通过电源线与电源匹配器26相连，所述单电极等离子体发生器位于罩壳29内，电源匹配器26、导布辊2和带有调速电机的导布辊21分别位于罩壳29的外部，且导布辊28和带有调速电机的导布辊21分别布置于罩壳29两侧且相互平行，罩壳29上开有供织物和电源线进出的孔洞。
在本发明的一种实施方式中，所述单电极等离子体发生器负极24为两块长方体铝合金块，单电极等离子体发生器正极25为套有玻璃管的铝合金管；单电极等离子体发生器负极24和单电极等离子体发生器正极25通过金属螺丝以及电极两端的四氟乙烯绝缘块和铝合金外套固定，组成单电极等离子体发生器。
在本发明的一种实施方式中，所述单电极等离子体发生器包括冷凝设备，所述冷凝设备包括冷凝水进水管(19)、冷凝管和冷凝水出水管(20)且三者首尾依次相连，所述冷水进水管(19)和冷水出水管(20)分别位于电极等离子体发生器的两端，所述冷凝管穿过电极等离子体发生器，防止电极过热。
在本发明的一种实施方式中，所述接枝气体管路14、接枝气体管路14上的电磁阀4和流量计5、第二管路16以及第三管路17都装有保温层，防止接枝单体气体冷凝。
在本发明的一种实施方式中，所述单电极等离子体发生器负极24中放置一铜管，铜管上开有小孔，作为气体的出气口18，所述出气口18位于单电极等离子体发生器正极25的上方，所述第三管路17中的气体通过单电极等离子体发生器负极上的出气口18进入单电极等离子体发生器。
在本发明的一种实施方式中，所述电源匹配器26通过电源线与电源相连，所述电源位于罩壳29的外部。
在本发明的一种实施方式中，所述加热设备10用于加热接枝单体使之气化，经过接枝气体管路14、第二管路16、第三管路17，进入单电极等离子体发生器；所述加热设备10与控温加热模块12相连，所述控温加热模块12包括加热电源和温度控制装置，用于提供热量并 控制加热温度。
在本发明的一种实施方式中，所述接枝罐8开有加液口13，用于将接枝单体加入接枝罐8。
在本发明的一种实施方式中，所述接枝罐8的加液口13处安装有测液位棒9，所述测液位棒9用于测定接枝液11的液位。
在本发明的一种实施方式中，所述罩壳29的材质优选为有机玻璃。
在本发明的一种实施方式中，所述织物与单电极等离子体发生器平行，当织物27置于导布辊上，并从单电极等离子体发生器下通过时，实现了大气等离子体对织物的连续处理。
在本发明的一种实施方式中，所述罩壳29上有排风口23，以及与排风口23相连的风扇22，用于剩余未反应的气体的收集。
在本发明的一种实施方式中，放电电极置于该玻璃罩内，便于收集废气，统一排出。
在本发明的一种实施方式中，仪器所用气体或者接枝单体的种类与织物处理的效果相对应，不同的织物整理效果，需要不同的气体或者接枝单体。
在本发明的一种实施方式中，当为抗菌整理时，所述载气为氦气或者氩气；所述反应气体为氨气或者氮气，或所述接枝单体为含氮的小分子有机单体，其中，所述含氮的小分子有机单体包括甲胺、乙二胺、1,2-丙二胺、炔丙胺、异丙胺、二异丙胺、正丙胺、二正丙胺等中的任一种。
在本发明的一种实施方式中，当为拒水拒油整理时，所述载气为氦气或者氩气；所述反应气体为四氟化碳，或者所述接枝单体为二氟乙烯、四氟乙烯、六氟乙烯等。
在本发明的一种实施方式中，当为阻燃整理时，所述载气为氦气或者氩气；所述反应气体为四氟化碳和甲烷的混合气体，或者所述接枝单体为丙烯酸。
在本发明的一种实施方式中，当为抗静电整理时，所述载气为氦气或者氩气；所述反应气体为二氧化硫，或者所述接枝单体为丙烯酸、乙烯基单体等。
在本发明的一种实施方式中，气体的流速可以通过流量计控制，以达到稳定的等离子体释放。
在本发明的一种实施方式中，接枝的时候，需要载体气体带着接枝单体进入放电装置，保证稳定的放电和等离子体输出。
在本发明的一种实施方式中，所述带有调速电机的导布辊上包括一速度开关，用于控制织物传送的速度。
此外，本发明还提供了一种大气压等离子接枝法对织物进行功能性整理的方法，所述方法在大气压等离子体设备上进行。
在本发明的一种实施方式中，所述方法的步骤为
(1)先打开等离子体设备的总电源开关，使设备通电；
(2)打开载体气体的气瓶，打开电磁阀和流量计，测试管路正常通气；
(3)当等离子体对织物进行功能整理所采用的单体为气体时，载体气体管路(1)的载体气体与反应性气体管路(2)的反应性气体在第一管路(15)中汇合，进入第三管路(17)，通过单电极等离子体发生器负极上的出气口(18)进入单电极等离子体发生器进行等离子体化；
当等离子体对织物进行功能整理所采用的单体为液体时，在接枝罐(8)中加入接枝单体，经过加热设备的加热使得接枝单体气化，经接枝气体管路(14)，并与载体气体管路(6)的气体在第二管路(16)中汇合，进入第三管路(17)，通过单电极等离子体发生器负极上的出气口(18)进入单电极等离子体发生器，进行等离子体化；
(4)打开导布辊电机并调整导布辊速率使得织物从单电极等离子体发生器下通过，实现大气等离子体对织物的功能性处理。
在本发明的一种实施方式中，所述功能性整理包括抗菌整理、拒水拒油整理、阻燃整理、抗静电整理等。
在本发明的一种实施方式中，当为抗菌整理时，所述载气为氦气或者氩气；所述反应气体为氨气和或者氮气；所述接枝单体为含氮的小分子有机单体，其中，所述含氮的小分子有机单体包括甲胺、乙二胺、1,2-丙二胺、炔丙胺、异丙胺、二异丙胺、正丙胺、二正丙胺等。
在本发明的一种实施方式中，当为拒水拒油整理时，所述载气为氦气或者氩气；所述反应气体为四氟化碳；所述接枝单体为二氟乙烯、四氟乙烯、六氟乙烯等氟碳化合物。
在本发明的一种实施方式中，当为阻燃整理时，所述载气为氦气或者氩气；所述反应气体为四氟化碳，或者所述接枝单体为丙烯酸。
在本发明的一种实施方式中，当为抗静电整理时，所述载气为氦气或者氩气；所述反应气体为二氧化硫，或者所述接枝单体为丙烯酸、乙烯基单体等。
在本发明的一种实施方式中，所述载体、反应气体、接枝单体的流量分别需根据整理的效果以及反应气体和单体气体等离子体化的条件而调节。
在本发明的一种实施方式中，所述加热杯的加热温度以接枝单体能够气化为准。
在本发明的一种实施方式中，当为抗菌整理时，等离子体化的单体在织物27表面重排、聚合，在织物表面引入含氮基团，经次氯酸钠溶液氯化后，赋予织物抗菌效果。
在本发明的一种实施方式中，等离子体化的操作参数为：载体气体流量为1-15L/min，单体气化温度为0-200℃，保温温度为0-200℃，流量为0.006-0.06L/min，电源功率为0-500W。
在本发明的一种实施方式中，所述织物传送的速度通过导布辊上的电机控制，其速度范围为0.001-0.1m/s。
与现有技术相比，本发明的有益效果是：
(1)通过本发明的大气压等离子体设备用等离子体对织物进行功能性处理，实现了织物无水或者少水的处理方法，无废水产生，环保，同时减轻废水处理负担。
(2)该设备改变现有的等离子体间歇式的处理方式，实现等离子体对织物的连续化加工处理。
(3)本发明功能性整理的效果可与化学法处理相媲美，但是较化学方法相比，更加环保。
(4)本发明的设备和方法在无水的条件下，实现了织物的功能性整理，这一处理过程反应迅速、耗时短、高效、环保、操作简单、处理效果均一、对织物的没有选择性以及不改变织物本身的性质。
附图说明
图1为本发明中等离子体机器的结构示意图；其中，1、载体气体管路，2、反应性气体管路，3、控制柜，4、电磁阀，5、流量计，6、载体气体管路，7、接枝仪，8、接枝罐，9、测液位棒，10、加热设备，11、接枝液体，12、控温加热模块，13、加液口，14、接枝气体管路，15、第一管路，16、第二管路，17、第三管路，18、出气口，19、冷凝水进水管，20、冷凝水出水管，21、带有调速电机的导布辊，22、风扇，23、排风口，24、单电极等离子体发生器负极，25、单电极等离子体发生器正极，26、电源匹配器，27、织物，28、导布辊，29、有机玻璃罩。
图2单电极等离子体发生器的结构示意图。
图3等离子体接枝处理前后棉织物表面元素的XPS谱图。
图4(a)等离子体沉积处理前(b)等离子体沉积处理后(c)等离子体沉积处理后并氯化的棉织物的SEM图片。
图5光栅测试等离子体沉积处理后织物表面损伤程度。
图6等离子体(a)处理时间和(b)功率对织物撕破强力的影响。
具体实施方式
实施例1
如图1-2所示，所述的大气压等离子体设备包括载体气体管路1、反应性气体管路2、载体气体管路6、接枝气体管路14、第一管路15、第二管路16、第三管路17、单电极等离子体发生器负极24和单电极等离子体发生器正极25，其中，第三管路17与由单电极等离子体发生器负极24和单电极等离子体发生器正极25组成的单电极等离子体发生器相连，所述第三管路17的气体为第一管路15的气体或第二管路16的气体汇合而成，所述第一管路15的气体由载体气体管路1的载体气体和反应性气体管路2的反应气体汇合而成，所述第二管路16的气体由载体气体管路6的载体气体和接枝气体管路14的接枝气体汇合而成；所述接枝气体管路14的另一端与接枝罐8相连，所述接枝罐8的外部安装有加热设备10，加热设备10与控温加热模块12相连，所述控温加热模块12包括加热电源和温度控制装置，接枝罐8的加液口13处设有测液位棒9，所述接枝气体管路14的接枝气体是接枝罐8内气化后的接枝单体得到的；所述载体气体管路1、反应性气体管路2、载体气体管路6和接枝气体管路14上均安装有电磁阀4和流量计5；所述由单电极等离子体发生器负极24和单电极等离子体发生器正极25组成的单电极等离子体发生器通过电源线与电源匹配器26相连，所述单电极等离子体发生器位于罩壳29内，电源、电源匹配器26、导布辊2和带有调速电机的导布辊21分别位于罩壳29的外部，且导布辊28和带有调速电机的导布辊21分别布置于罩壳29两侧且相互平行，罩壳29上开有供织物和电源线进出的孔洞，罩壳29上有排风口23，以及与排风口23相连的风扇22，用于剩余气体的收集；所述织物与单电极等离子体发生器平行，当织物27置于导布辊上，并从单电极等离子体发生器下通过时，实现了大气等离子体对织物的连续处理。
其中，所述单电极等离子体发生器负极24为两块长方体铝合金块，单电极等离子体发生器正极25为套有玻璃管的铝合金管；单电极等离子体发生器负极24和单电极等离子体发生器正极25通过金属螺丝以及电极两端的四氟乙烯绝缘块和铝合金外套固定，组成单电极等离子体发生器，所述单电极等离子体发生器负极24中放置一铜管，铜管上开有小孔，作为气体的出气口18，所述出气口18位于单电极等离子体发生器正极25的上方；所述单电极等离子体发生器包括冷凝设备，所述冷凝设备包括冷凝水进水管(19)、冷凝管和冷凝水出水管(20)且三者首尾依次相连，所述冷水进水管(19)和冷水出水管(20)分别位于电极等离子体发生器的两端，所述冷凝管穿过电极等离子体发生器，防止电极过热。
优选的，所述接枝气体管路14、接枝气体管路(14)上的电磁阀(4)和流量计(5)、 以及第三管路17上都装有保温层，防止接枝单体气体冷凝。
优选的，所述加热设备10用于加热接枝单体使之气化，进入接枝气体管路14，与载体气体管路6中的载体气体在第二管路16中汇合，进入第三管路17，通过单电极等离子体发生器负极上的出气口18进入由单电极等离子体发生器负极24和单电极等离子体发生器正极25组成的单电极等离子体发生器，等离子体化，对织物27进行处理。
优选的，所述罩壳29的材质优选为有机玻璃。
在打开各个管路的阀门和开关前，将接枝液11加入到接枝罐8中，打开控温加热模块12的加热电源和温度控制装置，用于提供热量并控制加热温度使得接枝液加热气化。
打开各个管路的阀门和开关，气化后的接枝单体进入接枝气体管路14，与载体气体管路6中的载体气体在第二管路16中汇合，进入第三管路17，通过单电极等离子体发生器负极上的出气口18进入由单电极等离子体发生器负极24和单电极等离子体发生器正极25组成的单电极等离子体发生器，进行等离子体化，对织物27进行功能性处理，当织物27置于导布辊上，并从单电极等离子体发生器下通过时，实现了大气等离子体对织物的连续处理。
综上，实现了大气等离子体对织物的连续处理，实现了织物的干法整理，无废水废液产生，从而实现织物的清洁整理。
实施例2：抗菌整理
抗菌整理的方法：
(1)先打开等离子体设备的总电源开关，使设备通电；
(2)在接枝罐中加入接枝单体1,2-丙二胺，经过加热设备10加热，使之气化，通过电磁阀4和流量计5，调节其流量为0.01L/min，然后，经接枝气体管路14，与载体气体管路6中的载体气体(氩气，流量为8L/min)在第二管路16中汇合，进入第三管路17，通过单电极等离子体发生器负极上的出气口18进入由单电极等离子体发生器负极24和单电极等离子体发生器正极25组成的单电极等离子体发生器，功率为300W，等离子体化；
(3)打开导布辊电机并调整导布辊速率为0.05m/s，使得棉织物从单电极等离子体发生器下通过，实现大气等离子体对织物的功能性处理。
等离子体化的单体在织物27表面重排、聚合，在织物表面引入含氮基团，经1.0wt％的次氯酸钠溶液氯化后，赋予织物抗菌效果。
含氮小分子有机单体等离子体处理后的织物表面XPS元素分析谱图如图3所示。从图3中可以看出，等离子体接枝法对棉织物处理后，棉织物表面含有氮元素。也就是说，含氮小 分子有机单体等离子体处理织物后，可以在织物表面引入氮元素。根据XPS测试结果，对织物表面元素含量的计算，结果如表1所示。从表1可知，等离子体沉积对棉织物处理之前，织物表面由C和O元素组成，含量分别为72.46％和27.54％，等离子体对棉织物处理之后，棉织物表面的元素组成为C、O和N，含量分别为68.70％、17.28％和14.02％，因此，含氮小分子有机单体等离子体沉积在棉织物表面上，从而使C和O元素的含量下降。
表1等离子体处理前后织物表面元素
Figure PCTCN2019129709-appb-000001
含氮小分子有机单体等离子体处理后的织物表面SEM图如图4所示。从图4中可以看出，与未经等离子体处理的棉织物相比，经等离子体处理后，棉纤维表面出现很多凹坑和网状结构，并且即使经过次氯酸钠氯化，这些凹坑和网状结构依然存在。从SEM图可以看出，含氮小分子有机单体等离子体对棉织物进行处理，对棉纤维有损伤，但损伤不大。通过光栅法测试了织物在等离子体处理后的损伤程度，如图5所示。从图5中的光栅法测试进一步证实了，与未处理的棉织物相比，等离子体对纤维的损伤尺寸为300-450nm。因此，含氮小分子有机单体等离子体对织物进行处理的损伤不明显。
图6是等离子处理中处理时间和功率对织物的撕破强力的影响的测试结果。从图中可以看出，处理时间在4min以内，功率在1400w以下，相比于未经等离子体处理的织物，等离子体处理后放的织物的撕破强力是增加的，说明等离子体沉积可增强织物的撕破强力，从而弥补织物因等离子体刻蚀引起的强力损失。
另外，通过AATCC 147-2016测试织物对金黄色葡萄球菌和大肠埃希氏菌的抗菌性能，在织物的下方和周围没有细菌滋生，可见，通过等离子体接枝法使含氮有机小分子单体在棉织物表面接枝，可以起到杀菌的作用。
实施例3：拒水整理
(1)先打开等离子体设备的总电源开关，使设备通电；
(2)在反应性气体管路2中通入四氟化碳，通过电磁阀4和流量计5，调节其流量为0.3L/min，然后，与载体气体管路1中的载体气体(氦气，流量为6L/min)在第一管路15中汇合，进入第三管路17，通过单电极等离子体发生器负极上的出气口18进入由单电极等 离子体发生器负极24和单电极等离子体发生器正极25组成的单电极等离子体发生器，功率为300W，等离子体化；
(3)打开导布辊电机并调整导布辊速率为0.05m/s，使得织物从单电极等离子体发生器下通过，实现大气等离子体对织物的功能性处理。
等离子体化的单体在织物27表面重排、聚合，在织物表面引入氟元素。对织物进行接触角测定：使用OCA40型视频接触角测量仪进行织物与水的接触角测试，水量为5μL，水滴与织物接触60s后读数。在同一样品的不同位置测量4次，取平均值。对棉织物洗前、洗15次后分别进行检测。洗前接触角可达148.7°，水洗15次后接触角为136.5°，达到了较好的拒水效果。
实施例4：阻燃整理
(1)先打开等离子体设备的总电源开关，使设备通电；
(2)在反应性气体管路2中通入四氟化碳和甲烷的混合气体，其中，四氟化碳的含量占总气体体积的50％，通过电磁阀4和流量计5，调节混合气体的流量为0.3L/min，然后，与载体气体管路1中的载体气体(氩气，流量为5L/min)在第一管路15中汇合，进入第三管路17，通过单电极等离子体发生器负极上的出气口18进入由单电极等离子体发生器负极24和单电极等离子体发生器正极25组成的单电极等离子体发生器，功率为400W，等离子体化；
(3)打开导布辊电机并调整导布辊速率为0.1m/s，使得织物从单电极等离子体发生器下通过，实现大气等离子体对织物的功能性处理。
等离子体化的单体在织物27表面重排、聚合，对整理后的织物用垂直燃烧法(GB/T20286-2006)点燃12s后测得极限氧指数(LOI)：26.3％，续燃时间：2s，损毁炭长：15.6mm；而未处理的织物的极限氧指数(LOI)：19.1％，续燃时间：9s，损毁炭长：30.5mm。
虽然本发明已以较佳实施例公开如上，但其并非用以限定本发明，任何熟悉此技术的人，在不脱离本发明的精神和范围内，都可做各种的改动与修饰，因此本发明的保护范围应该以权利要求书所界定的为准。

Claims (23)

  1. 一种大气压等离子接枝法对织物进行抗菌整理的方法，其特征在于，所述方法采用大气压等离子体设备直接对织物进行抗菌整理；所述大气压等离子体设备包括载体气体管路(1)、反应性气体管路(2)、载体气体管路(6)、接枝气体管路(14)、第一管路(15)、第二管路(16)、第三管路(17)、单电极等离子体发生器负极(24)和单电极等离子体发生器正极(25)，其中，第三管路(17)与由单电极等离子体发生器负极(24)和单电极等离子体发生器正极(25)组成的单电极等离子体发生器相连，所述第三管路(17)的气体为第一管路(15)的气体或第二管路(16)的气体汇合而成，所述第一管路(15)的气体由载体气体管路(1)的载体气体和反应性气体管路(2)的反应气体汇合而成，所述第二管路(16)的气体由载体气体管路(6)的载体气体和接枝气体管路(14)的接枝气体汇合而成；所述接枝气体管路(14)的另一端与接枝罐(8)相连，所述接枝罐(8)的外部安装有加热设备(10)，所述接枝气体管路(14)的接枝气体是接枝罐(8)内的接枝单体气化后得到的；所述载体气体管路(1)、反应性气体管路(2)、载体气体管路(6)和接枝气体管路(14)上均安装有电磁阀(4)和流量计(5)；
    所述由单电极等离子体发生器负极(24)和单电极等离子体发生器正极(25)组成的单电极等离子体发生器通过电源线与电源匹配器(26)相连，所述单电极等离子体发生器位于罩壳(29)内，电源匹配器(26)、导布辊(2)和带有调速电机的导布辊(21)分别位于罩壳(29)的外部，且导布辊(28)和带有调速电机的导布辊(21)分别布置于罩壳(29)两侧且相互平行，罩壳(29)上开有供织物和电源线进出的孔洞；
    所述方法包括以下步骤：
    (1)先打开等离子体设备的总电源开关，使设备通电；
    (2)在接枝罐中加入接枝单体，经过加热设备(10)加热，使之气化，通过电磁阀(4)和流量计(5)，调节其流量为0.006-0.06L/min，然后，经接枝气体管路(14)，与载体气体管路(6)中的载体气体在第二管路(16)中汇合，进入第三管路(17)，通过单电极等离子体发生器负极上的出气口(18)进入由单电极等离子体发生器负极(24)和单电极等离子体发生器正极(25)组成的单电极等离子体发生器，功率为300-500W，等离子体化；
    (3)打开导布辊电机并调整导布辊速率为0.001-0.1m/s，使得棉织物从单电极等离子体发生器下通过，实现大气等离子体对织物的抗菌处理；
    所述载气为氦气或者氩气；所述接枝单体为含氮的小分子有机单体，其中，所述含氮的小分子有机单体包括甲胺、乙二胺、1,2-丙二胺、炔丙胺、异丙胺、二异丙胺、正丙胺、二正丙胺中的任一种。
  2. 一种大气压等离子体设备，其特征在于，包括载体气体管路(1)、反应性气体管路(2)、载体气体管路(6)、接枝气体管路(14)、第一管路(15)、第二管路(16)、第三管路(17)、单电极等离子体发生器负极(24)和单电极等离子体发生器正极(25)，其中，第三管路(17)与由单电极等离子体发生器负极(24)和单电极等离子体发生器正极(25)组成的单电极等离子体发生器相连，所述第三管路(17)的气体为第一管路(15)的气体或第二管路(16)的气体汇合而成，所述第一管路(15)的气体由载体气体管路(1)的载体气体和反应性气体管路(2)的反应气体汇合而成，所述第二管路(16)的气体由载体气体管路(6)的载体气体和接枝气体管路(14)的接枝气体汇合而成；所述接枝气体管路(14)的另一端与接枝罐(8)相连，所述接枝罐(8)的外部安装有加热设备(10)，所述接枝气体管路(14)的接枝气体是接枝罐(8)内的接枝单体气化后得到的；所述载体气体管路(1)、反应性气体管路(2)、载体气体管路(6)和接枝气体管路(14)上均安装有电磁阀(4)和流量计(5)；
    所述由单电极等离子体发生器负极(24)和单电极等离子体发生器正极(25)组成的单电极等离子体发生器通过电源线与电源匹配器(26)相连，所述单电极等离子体发生器位于罩壳(29)内，电源匹配器(26)、导布辊(2)和带有调速电机的导布辊(21)分别位于罩壳(29)的外部，且导布辊(28)和带有调速电机的导布辊(21)分别布置于罩壳(29)两侧且相互平行，罩壳(29)上开有供织物和电源线进出的孔洞。
  3. 根据权利要求2所述的一种大气压等离子体设备，其特征在于，所述单电极等离子体发生器包括冷凝设备，所述冷凝设备包括冷凝水进水管(19)、冷凝管和冷凝水出水管(20)且三者首尾依次相连，所述冷水进水管(19)和冷水出水管(20)分别位于电极等离子体发生器的两端，所述冷凝管穿过电极等离子体发生器。
  4. 根据权利要求2或3所述的一种大气压等离子体设备，其特征在于，所述第三管路(17)中的气体通过单电极等离子体发生器负极上的出气口(18)进入单电极等离子体发生器。
  5. 根据权利要求2～4任一所述的一种大气压等离子体设备，其特征在于，所述接枝气体管路(14)、接枝气体管路(14)上的电磁阀(4)和流量计(5)、第二管路(16)以及第三管路(17)上装有保温层，防止接枝单体气体冷凝。
  6. 根据权利要求2～5任一所述的一种大气压等离子体设备，其特征在于，所述接枝罐(8)开有加液口(13)，用于将接枝单体加入接枝罐(8)。
  7. 根据权利要求2～6任一所述的一种大气压等离子体设备，其特征在于，所述单电极等离子体发生器负极(24)中放置一铜管，铜管上开有小孔，作为气体的出气口(18)，所述出气口(18)位于单电极等离子体发生器正极(25)的上方，所述第三管路(17)中的气体通 过单电极等离子体发生器负极上的出气口(18)进入单电极等离子体发生器。
  8. 根据权利要求2～7任一所述的一种大气压等离子体设备，其特征在于，所述电源匹配器(26)通过电源线与电源相连，所述电源位于罩壳(29)的外部。
  9. 根据权利要求2～8任一所述的一种大气压等离子体设备，其特征在于，所述加热设备(10)用于加热接枝单体使之气化，经过接枝气体管路(14)、第二管路(16)、第三管路(17)，进入单电极等离子体发生器；所述加热设备(10)与控温加热模块(12)相连，所述控温加热模块(12)包括加热电源和温度控制装置，用于提供热量并控制加热温度。
  10. 根据权利要求2～9任一所述的一种大气压等离子体设备，其特征在于，所述接枝罐(8)开有加液口(13)，用于将接枝单体加入接枝罐(8)；所述接枝罐(8)的加液口13处安装有测液位棒9，所述测液位棒9用于测定接枝液11的液位。
  11. 根据权利要求2～10任一所述的一种大气压等离子体设备，其特征在于，所述织物与单电极等离子体发生器平行，当织物(27)置于导布辊上，并从单电极等离子体发生器下通过时，实现了大气等离子体对织物的连续处理。
  12. 根据权利要求2～11任一所述的一种大气压等离子体设备，其特征在于，所述罩壳(29)上有排风口(23)，以及与排风口(23)相连的风扇(22)，用于剩余未反应的气体的收集。
  13. 一种大气压等离子接枝法对织物进行功能性整理的方法，其特征在于，所述方法在权利要求2～12任一所述的大气压等离子体设备上进行。
  14. 根据权利要求13所述的一种大气压等离子沉积法对织物进行功能性整理的方法，其特征在于，所述方法包括以下步骤：
    (1)先打开等离子体设备的总电源开关，使设备通电；
    (2)打开载体气体的气瓶，打开电磁阀和流量计，测试管路正常通气；
    (3)当等离子体对织物进行功能整理所采用的单体为气体时，载体气体管路(1)的载体气体与反应性气体管路(2)的反应性气体在第一管路(15)中汇合，进入第三管路(17)，通过单电极等离子体发生器负极上的出气口(18)进入单电极等离子体发生器进行等离子体化；
    当等离子体对织物进行功能整理所采用的单体为液体时，在接枝罐(8)中加入接枝单体，经过加热设备的加热使得接枝单体气化，经接枝气体管路(14)，并与载体气体管路(6)的气体在第二管路(16)中汇合，进入第三管路(17)，通过单电极等离子体发生器负极上的出气口(18)进入单电极等离子体发生器，进行等离子体化；
    (4)打开导布辊电机并调整导布辊速率使得织物从单电极等离子体发生器下通过，实现大气等离子体对织物的功能性处理。
  15. 根据权利要求14所述的一种大气压等离子接枝法对织物进行功能性整理的方法，其特征在于，所述反应气体为空气、氧气、氮气、氢气、氨气、二氧化碳、一氧化碳、四氟化碳、四氯化碳一种或几种；所述载气为氦气或氩气；所述接枝单体为乙烯基化合物、环氧化合物、饱和烃化合物、芳香族化合物或有机金属化合物。
  16. 根据权利要求14或15所述的一种大气压等离子接枝法对织物进行功能性整理的方法，其特征在于，所述功能性整理包括抗菌整理、拒水拒油整理、阻燃整理或抗静电整理。
  17. 根据权利要求16所述的一种大气压等离子接枝法对织物进行功能性整理的方法，其特征在于，当为抗菌整理时，所述载气为氦气或者氩气；所述反应气体为氨气和或者氮气；所述接枝单体为含氮的小分子有机单体，所述含氮的小分子有机单体为甲胺、乙二胺、1,2-丙二胺、炔丙胺、异丙胺、二异丙胺、正丙胺或二正丙胺。
  18. 根据权利要求16所述的一种大气压等离子接枝法对织物进行功能性整理的方法，其特征在于，当为拒水拒油整理时，所述载气为氦气或者氩气；所述反应气体为四氟化碳；所述接枝单体为二氟乙烯、四氟乙烯或六氟乙烯。
  19. 根据权利要求16所述的一种大气压等离子接枝法对织物进行功能性整理的方法，其特征在于，当为阻燃整理时，所述载气为氦气或者氩气；所述反应气体为四氟化碳，或者所述接枝单体为丙烯酸。
  20. 根据权利要求16所述的一种大气压等离子接枝法对织物进行功能性整理的方法，其特征在于，当为抗静电整理时，所述载气为氦气或者氩气；所述反应气体为二氧化硫，或者所述接枝单体为丙烯酸或乙烯基单体。
  21. 根据权利要求13-20任一所述的一种大气压等离子接枝法对织物进行功能性整理的方法，其特征在于，等离子体化的操作参数为：载体气体流量为1-15L/min，单体气化温度为0-200℃，保温温度为0-200℃，流量为0.006-0.06L/min，电源功率为0-500W。
  22. 根据权利要求13-21任一所述的一种大气压等离子接枝法对织物进行功能性整理的方法，其特征在于，所述织物传送的速度通过导布辊上的电机控制，其速度范围为0.001-0.1m/s。
  23. 权利要求2～12任一所述的一种大气压等离子体设备或权利要求1或13～22任一所述一种大气压等离子接枝法对织物进行功能性整理的方法在织物后整理领域中的应用。
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