CN103194886A - Preparation method of multi-phase heterogeneous visible light catalysis functional fabric - Google Patents
Preparation method of multi-phase heterogeneous visible light catalysis functional fabric Download PDFInfo
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Abstract
The invention relates to a preparation method of a multi-phase heterogeneous visible light catalysis functional fabric. The preparation method comprises the following steps of: (1) washing a fabric; (2) dropwise adding titanium tetraisopropoxide to deionized water, and heating the solution to 60-80 DEG C to react for 1-2 hours to obtain a solution A; (3) adding bismuth nitrate into a nitric acid solution and dropwise adding a wetting agent and a metal chelator to the solution to obtain a solution B; (4) adding metavanadate to the deionized water, heating the solution to 50-60 DEG C, and stirring the solution to obtain a solution C; (5) adding the solution B and the solution C to the solution A in sequence for reacting for 2-3 hours, and adjusting the pH of the solution mixture to alkalinity to obtain a heterogeneous photocatalyst finishing solution D; and (6) dipping the washed fabric to the finishing solution D, heating the finishing solution to 70-90 DEG C for reacting for 6-8 hours, and drying the fabric to obtain the multi-phase heterogeneous visible light catalysis functional fabric. The preparation method is simple and free of secondary pollution; and the functional fabric can be used for effectively purifying dyeing wastewater and air pollution under visible light irradiation.
Description
Technical field
The invention belongs to the Preparation of catalysts field, particularly a kind of preparation method of heterogeneous heterogeneous visible light catalytic function fabric.
Background technology
Along with the violent expansion of socioeconomic fast development and population, human demand to the energy increases considerably, and global environmental problem is also remarkable day by day.The utilization of solar energy exploitation seems particularly important for this reason, and is expected to become the effective means that solves environment and energy problem as the conductor photocatalysis technology of pith wherein.Be that the photodissociation water technology of clean Hydrogen Energy will thoroughly solve the crisis that fossil energy is exhausted and greenhouse effects bring with conversion of solar energy, and photocatalytic degradation is eliminated the approach that cheapness is feasible that toxic organic pollutant will become the solution environmental pollution.Therefore, the efficient visible light catalysis material of the synthetic reusable edible of design has become one of important topic that the research worker faces.
Using the most ripe photochemical catalyst at present is nano-TiO
2, but because the wideer ability that needs ultraviolet excitation just can possess oxidation of organic compounds of its energy gap has limited TiO
2In the application in environmental purification scope.Semiconductor compound photocatalyst can be formed with the semiconductor of location matches by two kinds, and it is compound to be generally the allos semiconductor.The coupling of this energy level makes semi-conductive energy gap reduce, and then the absorbing wavelength expanded range that makes composite semiconductor is to the visible region.On the one hand, the wide semiconductor of low energy gap can produce electron-hole pair under visible light, on the other hand, by carrying out compound with the semiconductor of the strong complementarity with different energy gaps, be conducive to separation of charge, suppress the compound of electronics-hole, improve quantum yield and catalytic efficiency.
In recent years, carried out both at home and abroad a series of on flexible fiber matrix load TiO
2The research of class photochemical catalyst utilizes three peacekeeping multilevel hierarchy features of fibrous material, broken through the restriction that the support type catalysis material is confined to inorganic material such as pottery, glass and metal for a long time.At the nano heterogeneous photochemical catalyst of flexible material interface assemble in situ, make up efficient visible light catalysis fabric, be research bright spot of the present invention.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of heterogeneous heterogeneous visible light catalytic function fabric, this method modern design, and the preparation method is simple, cost is low, does not increase new equipment, is easy to suitability for industrialized production; Fibrous raw material of the present invention source is wide, easily is processed into different shape, and is easy to use; Heterogeneous heterogeneous visible light catalytic function fabric of the present invention is effective to organic pollutant degradation, and non-secondary pollution can use for a long time.
The preparation method of a kind of heterogeneous heterogeneous visible light catalytic function fabric of the present invention comprises:
(1) fabric is cleaned 30-60min in organic solvent for ultrasonic, at 30-40 ℃ of dry 3-4h, in detergent, handle 25-35min, 60-65 ℃ of dry 5-10min, the fabric after obtaining handling in 40-45 ℃ again;
(2) titanium tetraisopropylate is added dropwise in the deionized water, is warming up to 60-80 ℃, stir 1-2h, get solution A; Wherein the volume ratio of titanium tetraisopropylate and deionized water is 1:9-11;
(3) bismuth nitrate is joined in the salpeter solution, drip wetting agent and metal-chelator, stir 20-30min, get solution B; Wherein the bismuth nitrate consumption is 0.5~5% of titanium tetraisopropylate consumption, and the wetting agent consumption is owf2%-5%;
(4) metavanadate is added in the deionized water, be warming up to 50-60 ℃, stir 25-30min, obtain solution C; Wherein the mol ratio of metavanadate and bismuth nitrate is 1:1;
(5) solution B and solution C are dropped in the solution A successively, stir 2-3h, it is 8-10 that alkaline agent is regulated the pH value, obtains nano heterogeneous photocatalysis finisher solution D;
(6) textile impregnation after will handling is in above-mentioned nano heterogeneous photocatalysis finisher solution D, and oil bath is warming up to 70-90 ℃, reaction 6-8h, and oven dry namely gets heterogeneous heterogeneous visible light catalytic function fabric.
Organic solvent is ethanol, ethyl acetate or acetone in the described step (1).
Fabric is non-weaving cloth, woven cloth or knitted cloth in the described step (1); Detergent is detergent Span-one.
Detergent is detergent Span-one (moral mulberry chemical industry) in the described step (1), detergent LS(dolantin chemical industry), detergent 6501(Basf) or detergent Kieralon OL(Basf).
The fiber of the fabric described in the described step (1) is cotton fiber, polyimide fiber, activated carbon fiber, polyester fiber, polypropylene fibre, bamboo fibre, the blend fibre of one or both in silk fiber, flax fibre, wool fibre, soybean fiber, milk protein fiber, the nylon fibre.
Wetting agent is JFC, tween or Qu Latong in the described step (3), and metal-chelator is disodium ethylene diamine tetraacetate, urea, citric acid, aminotriacetic acid, tartaric acid or polyacrylic acid; The concentration of metal-chelator in solution B is 0.05-0.4mol/L; The concentration of salpeter solution is 0.5-3mol/L.
Metavanadate is sodium metavanadate or ammonium metavanadate in the described step (4).
Drop rate is 2~4mL/min in the described step (5).
Alkaline agent in the described step (5) is ammoniacal liquor, NaOH or sodium carbonate.
Stir speed (S.S.) is 200~300rpm in described step (2)-(5).
In the described solution A of described step (2) in deionized water and the step (1) ratio of used fabric be respectively 50~70mL:1g; In the described solution B of step (3) in salpeter solution and the step (1) ratio of used fabric be 20~30mL:1g; In the described solution C of step (4) in deionized water and the step (1) ratio of used fabric be 20~30mL:1g.
Bake out temperature is 40-50 ℃ in the described step (6).
The heterogeneous heterogeneous visible light catalytic function fabric of the present invention's preparation can be applicable to environmental improvement fields such as printing-dying wastewater recycling, enterprise's sewage discharge processing, air pollution purification, has broad application prospects and market prospects.
The present invention is the pre-preparation nano-TiO under low temperature environment
2Colloidal sol by introducing the stabilizing solution of bismuth nitrate and metavanadate successively, forms BiVO
4/ TiO
2Nanometer mixed crystal solution, in the process that heats up with BiVO
4With TiO
2Carry out the crystal coupling, form hetero-junctions, promote TiO
2The separative efficiency of electron-hole pair.Adopt the growth in situ mode to carry out the load of photochemical catalyst on the flexible fabric surface, utilize the pH control technique to synthesize required BiVO
4With TiO
2Crystal formation.The present invention had both solved the dust pollution question of photochemical catalyst when air cleaning, can avoid the problem of photochemical catalyst reunion decrease in efficiency on flexible parent metal again; The photocatalyst of photocatalytic fiber fabric face has high-hydrophilic, has strong oxidizing property concurrently, and the pollutant on the surface of can effectively degrading keeps self cleaning, has antibacterial effect simultaneously, and harmful microorganism is effectively killed.
Beneficial effect
(1) photochemical catalyst modern design of the present invention, the preparation method is simple, cost is low, does not increase new equipment, is easy to suitability for industrialized production;
(2) fibrous raw material of the present invention is originated extensively, easily is processed into different shape, and is easy to use;
(3) fabric after the present invention handles can be by the quick degradation of dye waste water of photocatalysis or toxic gas under the visible light condition, and it is become nontoxic material;
(4) heterogeneous heterogeneous visible light catalytic function fabric of the present invention is effective to organic pollutant degradation, and non-secondary pollution can use for a long time.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
(1) wool fabric surface preparation
With acetone ultrasonic cleaning wool fabric (1g) 30min, 30 ℃ of dry 3h, again at efficient detergent Kieralon OL(Basf) in handle 25min in 40 ℃, 60 ℃ of dry 10min obtain the preliminary treatment wool fabric;
(2) preparation of solution A
The 6mL titanium tetraisopropylate is dropwise joined in the 60mL deionized water, be warming up to 70 ℃, stir 1h with the speed of 300rpm and get solution A;
(3) preparation of solution B
The 0.12g bismuth nitrate is joined in the 30mL salpeter solution that concentration is 2mol/L, and drips 0.05g JFC(fatty alcohol-polyoxyethylene ether) and the 0.55g disodium ethylene diamine tetraacetate, stir 30min in 300rpm, get solution B;
(4) preparation of solution C
The 0.03g ammonium metavanadate is joined in the 20mL deionized water, be warming up to 60 ℃, stir 25min in 300rpm, to the solution homogeneous transparent, obtain solution C;
(5) preparation of dressing liquid D
Solution B and solution C are slowly dropped in the solution A successively, and the control drop rate is 3mL/min, and 300rpm stirs 1h, regulates pH=9 by NaOH, obtains nano heterogeneous photochemical catalyst finisher solution D;
(6) the back arrangement of fabric
The preliminary treatment wool fabric that step (1) is obtained is impregnated among the above-mentioned nano heterogeneous finisher solution D, and oil bath is warming up to 90 ℃, and reaction 8h finally by 50 ℃ of oven dry, obtains waste water from dyestuff and purifies wool fabric.
Water environment purification wool fabric and common active carbon waste water decoloring material that the present invention is made are respectively charged in the purification of waste water device of same model, be light source with the 350W xenon lamp, degraded concentration is the waste water from dyestuff of 50mg/L, absorbance by waste water from dyestuff before and after the measurement of ultraviolet-visible spectrophotometer degraded, and calculate its residual concentration, draw the purifying rate of waste water from dyestuff, its result is as follows:
Embodiment 2
(1) surface of cotton fabric preliminary treatment
With ethanol ultrasonic cleaning COTTON FABRIC (1g) 40min, 30 ℃ of dry 3h, again in efficient detergent Span-one (moral mulberry chemical industry) solution 45 ℃ handle 25min, 65 ℃ of dry 5min obtain the preliminary treatment COTTON FABRIC;
(2) preparation of solution A
The 5.5mL titanium tetraisopropylate dropwise is added in the 55mL deionized water, is warming up to 70 ℃, stir 2h with the speed of 250rpm and get solution A;
(3) preparation of solution B
The 0.1g bismuth nitrate is joined in the 20mL salpeter solution that concentration is 1.5mol/L, and drip 0.05g Triton X-100 and 0.55g disodium ethylene diamine tetraacetate, stir 30min in 250rpm, get solution B;
(4) preparation of solution C
The 0.025g ammonium metavanadate is joined in the 20mL deionized water, stir 25min in 250rpm, to the solution homogeneous transparent, obtain solution C;
(5) preparation of dressing liquid D
Solution B and solution C are slowly dropped in the solution A successively, and the control drop rate is 2mL/min, and 250rpm stirs 1h, regulates pH=10 by NaOH, obtains nano heterogeneous photochemical catalyst finisher solution D;
(6) the back arrangement of fabric
The preliminary treatment COTTON FABRIC that step (1) is obtained is impregnated among the above-mentioned nano heterogeneous finisher solution D, and oil bath is warming up to 90 ℃, and reaction 8h finally by 45 ℃ of oven dry, obtains waste water from dyestuff and purifies COTTON FABRIC.
Water environment purification function COTTON FABRIC and common active carbon waste water decoloring material that the present invention is made are respectively charged in the purification of waste water device of same model, be light source with the 350W xenon lamp, degraded concentration is the waste water from dyestuff of 50mg/L, absorbance by waste water from dyestuff before and after the measurement of ultraviolet-visible spectrophotometer degraded, and calculate its residual concentration, draw the purifying rate of waste water from dyestuff, its result is as follows:
Embodiment 3
(1) sodolin surface preparation
With acetone ultrasonic cleaning sodolin (1g) 60min, 30 ℃ of dry 3h, again at efficient detergent LS(dolantin chemical industry) in the solution 40 ℃ handle 25min down, 60 ℃ of dry 10min obtain the preliminary treatment sodolin;
(2) preparation of solution A
The 6mL titanium tetraisopropylate is dropwise joined in the 65mL deionized water, be warming up to 65 ℃, stir 1h with the speed of 200rpm and get solution A;
(3) preparation of solution B
The 0.12g bismuth nitrate is joined in the 30mL salpeter solution that concentration is 2mol/L, and drips 0.05g JFC(fatty alcohol-polyoxyethylene ether) and the 0.55g disodium ethylene diamine tetraacetate, stir 30min in 200rpm, get solution B;
(4) preparation of solution C
The 0.03g ammonium metavanadate is joined in the 30mL deionized water, stir 30min in 200rpm, to the solution homogeneous transparent, obtain solution C;
(5) preparation of dressing liquid D
Solution B and solution C are slowly dropped in the solution A successively, and the control drop rate is 4mL/min, and 200rpm stirs 2h, regulates pH=9 by NaOH again, obtains nano heterogeneous photochemical catalyst finisher solution D;
(6) the back arrangement of fabric
The preliminary treatment sodolin that step (1) is obtained is impregnated among the above-mentioned nano heterogeneous finisher solution D, and oil bath is warming up to 90 ℃, and reaction 8h finally by 50 ℃ of oven dry, obtains waste water from dyestuff and purifies sodolin.
Water environment purification function sodolin and common active carbon waste water decoloring material that the present invention is made are respectively charged in the purification of waste water device of same model, be light source with the 350W xenon lamp, degraded concentration is the waste water from dyestuff of 50mg/L, absorbance by waste water from dyestuff before and after the measurement of ultraviolet-visible spectrophotometer degraded, and calculate its residual concentration, draw the purifying rate of waste water from dyestuff, its result is as follows:
Claims (10)
1. the preparation method of a heterogeneous heterogeneous visible light catalytic function fabric comprises:
(1) fabric is cleaned 30-60min in organic solvent for ultrasonic, at 30-40 ℃ of dry 3-4h, in detergent, handle 25-35min, 60-65 ℃ of dry 5-10min, the fabric after obtaining handling in 40-45 ℃ again;
(2) titanium tetraisopropylate is added dropwise in the deionized water, is warming up to 60-80 ℃, stir 1-2h, get solution A; Wherein the volume ratio of titanium tetraisopropylate and deionized water is 1:9-11;
(3) bismuth nitrate is joined in the salpeter solution, drip wetting agent and metal-chelator, stir 20-30min, get solution B; Wherein the bismuth nitrate consumption is 0.5~5% of titanium tetraisopropylate consumption, and the wetting agent consumption is owf2%-5%;
(4) metavanadate is added in the deionized water, be warming up to 50-60 ℃, stir 25-30min, obtain solution C; Wherein the mol ratio of metavanadate and bismuth nitrate is 1:1;
(5) solution B and solution C are dropped in the solution A successively, stir 1-3h, it is 8-10 that alkaline agent is regulated the pH value, obtains nano heterogeneous photocatalysis finisher solution D;
(6) textile impregnation after will handling is in above-mentioned nano heterogeneous photocatalysis finisher solution D, at 70-90 ℃, and reaction 6-8h, oven dry namely gets heterogeneous heterogeneous visible light catalytic function fabric.
2. the preparation method of a kind of heterogeneous heterogeneous visible light catalytic function fabric according to claim 1 is characterized in that: organic solvent is ethanol, ethyl acetate or acetone in the described step (1); Fabric is non-weaving cloth, woven cloth or knitted cloth; Detergent is detergent Span-one, detergent LS, detergent 6501 or detergent Kieralon OL.
3. the preparation method of a kind of heterogeneous heterogeneous visible light catalytic function fabric according to claim 1, it is characterized in that: the fiber of the fabric described in the described step (1) is cotton fiber, polyimide fiber, activated carbon fiber, polyester fiber, polypropylene fibre, bamboo fibre, the blend fibre of one or both in silk fiber, flax fibre, wool fibre, soybean fiber, milk protein fiber, the nylon fibre.
4. the preparation method of a kind of heterogeneous heterogeneous visible light catalytic function fabric according to claim 1, it is characterized in that: wetting agent is JFC, tween or Qu Latong in the described step (3), and metal-chelator is disodium ethylene diamine tetraacetate, urea, citric acid, aminotriacetic acid, tartaric acid or polyacrylic acid; The concentration of metal-chelator in solution B is 0.05-0.4mol/L; The concentration of salpeter solution is 0.5-3mol/L.
5. the preparation method of a kind of heterogeneous heterogeneous visible light catalytic function fabric according to claim 1 is characterized in that: metavanadate is sodium metavanadate or ammonium metavanadate in the described step (4).
6. the preparation method of a kind of heterogeneous heterogeneous visible light catalytic function fabric according to claim 1 is characterized in that: drop rate is 2-4mL/min in the described step (5).
7. the preparation method of a kind of heterogeneous heterogeneous visible light catalytic function fabric according to claim 1, it is characterized in that: the alkaline agent in the described step (5) is ammoniacal liquor, NaOH or sodium carbonate.
8. the preparation method of a kind of heterogeneous heterogeneous visible light catalytic function fabric according to claim 1 is characterized in that: stir speed (S.S.) is 200~300rpm in described step (2)-(5).
9. the preparation method of a kind of heterogeneous heterogeneous visible light catalytic function fabric according to claim 1 is characterized in that: in the described solution A of described step (2) in deionized water and the step (1) ratio of used fabric be respectively 50~70mL:1g; In the described solution B of step (3) in salpeter solution and the step (1) ratio of used fabric be 20~30mL:1g; In the described solution C of step (4) in deionized water and the step (1) ratio of used fabric be 20~30mL:1g.
10. the preparation method of a kind of heterogeneous heterogeneous visible light catalytic function fabric according to claim 1 is characterized in that: bake out temperature is 40-50 ℃ in the described step (6).
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CN105170183A (en) * | 2015-09-16 | 2015-12-23 | 天津工业大学 | Wool fiber metal complex photocatalyst and preparation method thereof |
CN106480721A (en) * | 2016-10-17 | 2017-03-08 | 盐城工学院 | Visible light catalytic function fabric and preparation method thereof |
CN111097521A (en) * | 2019-12-24 | 2020-05-05 | 南通天虹银海实业有限公司 | Preparation method of yarn based on bismuth vanadate photocatalytic function |
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