CN102505454B - Low-temperature in-situ preparation method based on Bi series photocatalytic semiconductor functional fabric - Google Patents
Low-temperature in-situ preparation method based on Bi series photocatalytic semiconductor functional fabric Download PDFInfo
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- CN102505454B CN102505454B CN 201110329511 CN201110329511A CN102505454B CN 102505454 B CN102505454 B CN 102505454B CN 201110329511 CN201110329511 CN 201110329511 CN 201110329511 A CN201110329511 A CN 201110329511A CN 102505454 B CN102505454 B CN 102505454B
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Abstract
The invention relates to a low-temperature in-situ preparation method based on a Bi series photocatalytic semiconductor functional fabric. The method comprises the following steps of: (1) performing ultrasonic cleaning on a fabric by using an organic solvent, and treating in a high-efficiency detergent to obtain a treated fabric; (2) adding bismuth nitrate and ethylene diamine tetraacetic acid into an alkaline buffer solution respectively in an inert environment, dripping a wetting agent to obtain a solution A, adding sodium metavanadate into an alkaline buffer solution in an inert environment, and adding a solution of sodium hydroxide and deionized water during stirring to obtain a solution B; (3) adding the solution B into the solution A dropwise to obtain a photocatalytic precursor solution; and (4) impregnating the treated fabric obtained in the step (1) in the photocatalytic precursor solution, drying, treating in boiling water, and finally oven-drying to obtain a product. The preparation method is simple and low in cost, and can be industrially produced easily; and the flexible photocatalytic environment purification material has a good wastewater treatment effect and can beused for a long time, and secondary pollution is avoided.
Description
Technical field
The invention belongs to the preparation field of photocatalysis environmental purification function fabric, particularly relating to a kind of is the low temperature in-situ growth method of photocatalytic semiconductor function fabric based on Bi.
Background technology
Water environment is an important component part of natural environment.At the earth's surface, coverage of water account for earth surface long-pending 71%, wherein available terrestrial water only accounts for 2.72% of Total Water, once the someone predicted, after energy crisis, the maximum natural crisis that the mankind will face is exactly water resources crisis.The deterioration of water environment, the shortage of water resource have become the focus that countries in the world are paid close attention to.As the valuable source that the mankind depend on for existence, the improvement of water environment has become the important topic that the mankind need to be resolved hurrily.
According to China Environmental State Bulletin; the section testing result of the main water system of China shows; have only 40% section to reach or be better than the III class of country's " ground water environment QUALITY STANDARD "; and the water quality of 60% section surpasses the IV class; lost the function as the drinking water source; the unbalance serious policy that restricts China's sustainable development of aquatic attitude, this singly is not the environmental resource crisis of China, global environment crisis of resource especially.
Dyestuff is as a kind of important fine chemical product, and is closely related with human clothing, food, lodging and transportion--basic necessities of life, and along with the fast development of dyeing, the dyeing waste water of supervening has also become one of current topmost pollution source of water body.At present, China produces dyestuff per year and surpasses 900,000 tons, occupies first place in the world, and accounts for 45% of Gross World Product.And in the production process of dyestuff, 1 ton of dyestuff of every output has at least 2% can run off with waste water, and the dyestuff loss amount then reaches 10%～15% in dyeing process.These dyestuffs are generally the organic compound of difficult degradation, life period in water is long, pollution range is wide, generation harm is big, intractability is high, water quality characteristic all shows as high concentration, high chroma, high COD and BOD value, and its relevant improvement technology is the difficult point place of wastewater treatment always.
At present, the method that is usually used in dye wastewater treatment both at home and abroad mainly contains: biological treatment, chemical flocculation, chemical oxidization method, absorption method and electrochemical process etc.; And also have some novel wastewater processing technology researchs comparatively active in recent years, as supercritical water oxidation technology, nonthermal plasma chemistry technology, ultrasonic technology, abstraction technique, photocatalysis technology and fenton oxidation technology etc.But there is the manufacturing technique complexity in above method, cost is higher and defective such as the use of can not regenerating, and is unfavorable for reclaiming, and influences sustainable development.In view of flexible parent metal (fibrous material) has big, the easy machine-shaping of surface area, easy enrichment pollutant and dilution catabolite property as carrier, photochemical catalyst is loaded on the flexible parent metal the flexible sewage purification material of preparation can effectively improve the ability of sewage disposal, and with low cost.The preparation method has at present: padding method and coating.These two kinds of methods exist photochemical catalyst and are coated by adhesive, serious, the problems such as catalytic efficiency is low, the easy photooxidative degradation of flexible parent metal of reuniting.Owing to the flexible parent metal non-refractory, limited photochemical catalyst and be deposited on the use of carrying out the crystal formation conversion method on the flexible parent metal again.
Summary of the invention
It is the low temperature in-situ growth method of photocatalytic semiconductor function fabric based on Bi that technical problem to be solved by this invention provides a kind of, this method is simple, and cost is low, non-secondary pollution, be easy to suitability for industrialized production, the flexible water environment scavenging material of gained can effectively purify dyeing waste water.
A kind of low temperature in-situ growth method that is the photocatalytic semiconductor function fabric based on Bi of the present invention comprises:
(1) preliminary treatment of fabric:
With organic solvent ultrasonic cleaning fabric 30～60min, 20～30 ℃ of drying 10～12h, in efficient detergent, handle 15～25min, 80～85 ℃ of drying 20～30min, the fabric after obtaining handling under 40～45 ℃ again;
(2) under inert environments, be that 1: 2 bismuth nitrate and disodium ethylene diamine tetraacetate adds respectively in the alkaline buffer with mol ratio, drip wetting agent, stir 20～30min in 200～300rpm, obtain solution A;
Under inert environments, will add in the alkaline buffer with the sodium metavanadate of the identical molal quantity of bismuth nitrate in the solution A, 200～300rpm stirs 5～10min, and dropwise adds sodium hydroxide solution and deionized water successively in whipping process, obtains solution B;
(3) preparation of LOC dressing liquid:
Solution B dropwise is added in the solution A, and the control transfer rate is 1～1.5ml/min, is uniformly mixed to form dressing liquid LOC, and place water-bath, be warming up to 80～95 ℃ from room temperature, the control heating rate obtains photocatalysis precursor solution (LOC dressing liquid) at 2～3 ℃/min;
(4) post processing of fabric face in-situ deposition and water environment purification function fabric:
Textile impregnation after the processing that step (1) is obtained reacts 8～12h in above-mentioned photocatalysis precursor solution, 65～70 ℃ of oven dry down, in 90～100 ℃ of boiling water, handle 1～2h then afterwards, remove the redundant adsorption particle at fabric face, at last in 40～50 ℃ of oven dry, namely.
Fabric described in the step (1) is non-weaving cloth, woven cloth or knitted cloth.
The fiber of above-mentioned fabrics is cotton fiber, polyimide fiber, activated carbon fiber, polyester fiber, polypropylene fibre, bamboo fibre, one or both blend fibres in silk fiber, flax fibre, wool fibre, soybean fiber, milk protein fiber, the nylon fibre.
Efficient detergent described in the step (1) is detergent Span-one (moral mulberry chemical industry), detergent LS (dolantin chemical industry), detergent 6501 (Basf) or detergent Kieralon OL (Basf).
Organic solvent described in the step (1) is hydro carbons or halogenated hydrocarbon organic solvents such as ethanol, ethyl acetate or acetone.
Described inert environments in the step (2) is nitrogen or argon shield environment.
Alkaline buffer described in the step (2) is that volume ratio is the mixed solution of the mixed solution of 3: 2 0.2mol/L sodium hydrogen phosphate and 0.2mol/L sodium dihydrogen phosphate, 0.2mol/L sodium hydrogen phosphate that volume ratio is 3: 2 and 0.1mol/L citric acid or 0.2mol/L NaOH that volume ratio is 3: 2 and the mixed solution of 0.2mol/L potassium dihydrogen phosphate.
Wetting agent described in the step (2) is JFC (fatty alcohol-polyoxyethylene ether), tween or Qu Latong (Triton X-100), and consumption is: owf 2%～6%.
Naoh concentration described in the step (2) is 0.5～2mol/L.
The ratio of used fabric is 40～60ml: 1g in alkaline buffer in the described solution A of step (2) and the step (1); The ratio of used fabric is respectively 40～60mL in solution B neutral and alkali buffer solution, sodium hydroxide solution and deionization and the step (1): 1g, 5～15ml: 1g and 5～15ml: 1g.
The present invention on fabric, had both solved the difficult recovery problem of the pollution of photochemical catalyst when wastewater treatment with the semi-conductor nano particles in-situ deposition, can avoid the problem of photochemical catalyst reunion decrease in efficiency on flexible parent metal again; The photo-catalyst film on flexible photocatalysis surrounding purifying material surface has high-hydrophilic, can form antifogging coating, simultaneously because its powerful oxidation, the oxidable pollutant that falls the surface keeps self cleaning, and flexible material can pass through the coloured dyestuff of photocatalytic degradation under visible light, and it is become the material of non-toxic, colorless, flexible photocatalysis surrounding purifying material good waste water treatment effect of the present invention, non-secondary pollution can use for a long time.
The surrounding purifying material 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 photocatalytic semiconductor by the synthetic Bi of original position on fabric directly, at textile surface generation crystal transfer, obtains efficient long-wave band efficiency of light absorption, prepares flexible photocatalysis surrounding purifying material.
Beneficial effect
(1) preparation method of the present invention 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) flexible photocatalysis surrounding purifying material good waste water treatment effect of the present invention, 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 soln ultrasonic cleaning wool fabric (1g) 30min, 20 ℃ of dry 10h, in efficient detergent KieralonOL (Basf) solution, handle 15min, 80 ℃ of dry 30min under 40 ℃ again;
(2) preparation of solution A
Under nitrogen environment, get the 0.005mol bismuth nitrate and the 0.010mol disodium ethylene diamine tetraacetate adds respectively in the 50ml phosphate buffer solution, and drip relative fabric and weigh 2% wetting agent Tween 80,200rpm stirs 30min;
(3) preparation of solution B
Under nitrogen environment, get the 0.005mol sodium metavanadate and add in the 50ml phosphate buffer solution, 200rpm stirs 5min, and dropwise adds 10ml sodium hydroxide solution (1.5mol/L) in whipping process, and the 10ml deionized water obtains settled solution;
(4) preparation of LOC dressing liquid
Solution B dropwise is added in the solution A, and control speed is 1ml/min, is uniformly mixed to form dressing liquid LOC, and places water-bath, is warming up to 90 ℃ from room temperature, and the control heating rate is 2 ℃/min, obtains the photocatalysis precursor solution;
(5) will be impregnated into through the wool fabric that step (1) is handled in the LOC dressing liquid of step (4) and react 8h, afterwards 65 ℃ of oven dry down;
(6) post processing of water environment purification function fabric
Fabric after step (5) oven dry is handled 1h in 100 ℃ of boiling water, remove the redundant adsorption particle at fabric face, again through 50 ℃ of oven dry, obtain water environment and purify wool fabric.
Water environment purification function 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, to under identical conditions: comprise the space, colorful wastewater concentration, time compare test, and its result is as follows:
Embodiment 2
(1) surface of cotton fabric preliminary treatment
With ethyl acetate ultrasonic cleaning COTTON FABRIC (1g) 50min, 30 ℃ of dry 12h, handle 25min, 85 ℃ of dry 20min down for 45 ℃ at efficient detergent KieralonOL (Basf) solution again;
(2) preparation of solution A
Under ar gas environment, get the 0.006mol bismuth nitrate and the 0.011mol disodium ethylene diamine tetraacetate adds respectively in the 50ml phosphate buffer solution, and drip relative fabric and weigh 2% wetting agent Tween 80,200rpm stirs 30min;
(3) preparation of solution B
Under ar gas environment, get the 0.006mol sodium metavanadate and add in the 50ml phosphate buffer solution, 200rpm stirs 5min, and dropwise adds 9ml sodium hydroxide solution (1.0mol/L) in whipping process, and the 9ml deionized water obtains settled solution;
(4) preparation of LOC dressing liquid
Solution B dropwise is added in the solution A, and control speed is 1ml/min, is uniformly mixed to form dressing liquid LOC, and places water-bath, is warming up to 90 ℃ from room temperature, and the control heating rate is 3 ℃/min, obtains the photocatalysis precursor solution;
(5) will be impregnated into through the COTTON FABRIC that step (1) is handled in the LOC dressing liquid of step (4) and react 10h, afterwards 65 ℃ of oven dry down;
(6) post processing of water environment purification function fabric
COTTON FABRIC after step (5) oven dry is handled 1h in 90 ℃ of boiling water, remove the redundant adsorption particle at fabric face, again through 40 ℃ of oven dry, obtain water environment and purify 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, and under identical conditions: comprise the space, colorful wastewater concentration, time compare test, and its result is as follows:
Embodiment 3
(1) sodolin surface preparation
With acetone soln ultrasonic cleaning sodolin (1g) 60min, 30 ℃ of dry 10h, handle 30min, 85 ℃ of dry 20min down for 45 ℃ at efficient detergent KieralonOL (Basf) solution again;
(2) preparation of solution A
Under nitrogen environment, get the 0.005mol bismuth nitrate and the 0.012mol disodium ethylene diamine tetraacetate adds respectively in the 60ml phosphate buffer solution, and drip relative fabric and weigh 5% Qu Latong, 200rpm stirs 30min;
(3) preparation of solution B
Under nitrogen environment, get the 0.005mol sodium metavanadate and add in the 60ml phosphate buffer solution, 200rpm stirs 5min, and dropwise adds 9ml sodium hydroxide solution (0.5mol/L) in whipping process, and the 9ml deionized water obtains settled solution;
(4) preparation of LOC dressing liquid
Solution B dropwise is added in the solution A, and control speed is 2ml/min, is uniformly mixed to form dressing liquid LOC, and places water-bath, is warming up to 90 ℃ from room temperature, and the control heating rate is 3 ℃/min, obtains the photocatalysis precursor solution;
(5) will be impregnated into through the sodolin that step (1) is handled in the LOC dressing liquid of step (4) and react 12h, afterwards 65 ℃ of oven dry down;
(6) post processing of water environment purification function fabric
Sodolin after step (5) oven dry is handled 1h in 90 ℃ of boiling water, remove the redundant adsorption particle at fabric face, again through 40 ℃ of oven dry, obtain water environment and purify 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, to under identical conditions: comprise the space, colorful wastewater concentration, time compare test, and its result is as follows:
Claims (9)
1. low temperature in-situ growth method that is the photocatalytic semiconductor function fabric based on Bi comprises:
(1) with organic solvent ultrasonic cleaning fabric 30～60min, 20～30 ℃ of drying 10～12h handle 15～25min, 80～85 ℃ of drying 20～30min, the fabric after obtaining handling under 40～45 ℃ again in efficient detergent;
(2) under inert environments, be that bismuth nitrate and the disodium ethylene diamine tetraacetate of 1:2 adds respectively in the alkaline buffer with mol ratio, drip wetting agent, stir 20～30min in 200～300rpm, obtain solution A;
Under inert environments, will add in the alkaline buffer with the sodium metavanadate of the identical molal quantity of bismuth nitrate in the solution A, 200～300rpm stirs 5～10min, and dropwise adds sodium hydroxide solution and deionized water successively in whipping process, obtains solution B;
(3) solution B dropwise is added in the solution A, the control transfer rate is 1～1.5ml/min, is uniformly mixed to form dressing liquid LOC, and place water-bath, be warming up to 80～95 ℃ from room temperature, the control heating rate obtains the photocatalysis precursor solution at 2～3 ℃/min;
(4) textile impregnation after the processing that step (1) is obtained reacts 8～12h in above-mentioned photocatalysis precursor solution, 65～70 ℃ of oven dry down, handles 1～2h then in 90～100 ℃ of boiling water, at last in 40～50 ℃ of oven dry, namely afterwards.
2. a kind of low temperature in-situ growth method that is the photocatalytic semiconductor function fabric based on Bi according to claim 1, it is characterized in that: the fabric described in the step (1) is non-weaving cloth, woven cloth or knitted cloth.
According to claim 1 a kind of be the low temperature in-situ growth method of photocatalytic semiconductor function fabric based on Bi, it is characterized in that: the efficient detergent described in the step (1) is detergent Span-one, detergent LS, detergent 6501 or detergent Kieralon OL.
4. a kind of low temperature in-situ growth method that is the photocatalytic semiconductor function fabric based on Bi according to claim 1, it is characterized in that: the organic solvent described in the step (1) is ethanol, ethyl acetate or acetone.
5. a kind of low temperature in-situ growth method that is the photocatalytic semiconductor function fabric based on Bi according to claim 1, it is characterized in that: the described inert environments in the step (2) is nitrogen or argon shield environment.
6. a kind of low temperature in-situ growth method that is the photocatalytic semiconductor function fabric based on Bi according to claim 1 is characterized in that: the alkaline buffer described in the step (2) is that volume ratio is the mixed solution of the mixed solution of the 0.2mol/L sodium hydrogen phosphate of 3:2 and 0.2mol/L sodium dihydrogen phosphate, 0.2mol/L sodium hydrogen phosphate that volume ratio is 3:2 and 0.1mol/L citric acid or 0.2mol/L NaOH that volume ratio is 3:2 and the mixed solution of 0.2mol/L potassium dihydrogen phosphate.
7. a kind of low temperature in-situ growth method that is the photocatalytic semiconductor function fabric based on Bi according to claim 1, it is characterized in that: the wetting agent described in the step (2) is JFC, tween or Qu Latong, and consumption is: owf2%～6%.
8. a kind of low temperature in-situ growth method that is the photocatalytic semiconductor function fabric based on Bi according to claim 1, it is characterized in that: the naoh concentration described in the step (2) is 0.5～2mol/L.
9. a kind of low temperature in-situ growth method that is the photocatalytic semiconductor function fabric based on Bi according to claim 1, it is characterized in that: the ratio of used fabric is 40～60ml:1g in the alkaline buffer in the described solution A of step (2) and the step (1); The ratio of used fabric is respectively 40～60ml in solution B neutral and alkali buffer solution, sodium hydroxide solution and deionized water and the step (1): 1g, 5～15ml:1g and 5～15ml:1g.
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| CN102912648B (en) * | 2012-11-02 | 2015-04-22 | 东华大学 | Preparation method for fiber-based activate core-shell micro-nano structure environment purifying material |
| CN103103743B (en) * | 2013-01-29 | 2015-02-25 | 东华大学 | Preparation method of interface plasma modified and amphiphilic fiber-based purifying material |
| CN107345340A (en) * | 2017-07-24 | 2017-11-14 | 厦门盛方生态技术有限公司 | A kind of production method of bamboo fibre and ramee composite mattress |
| CN110184818A (en) * | 2019-05-31 | 2019-08-30 | 云南浩祥服饰有限公司 | A kind of no-iron treatment method of cotton shirt |
| CN110670344B (en) * | 2019-10-16 | 2020-07-17 | 西北大学 | Super-hydrophobic flexible fabric with photocatalysis and oil-water separation performances and preparation method and application thereof |
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| JP2004330047A (en) * | 2003-05-06 | 2004-11-25 | Univ Kanazawa | Metal or metal oxide-carrying bismuth vanadate photocatalyst for photodecomposition of endocrine disruptor |
| CN1683074A (en) * | 2005-03-11 | 2005-10-19 | 南京大学 | Process for preparing visible light responding photo catalytic film layer |
| CN101413212B (en) * | 2008-11-27 | 2011-03-16 | 东华大学 | Method for preparing air self-purifying function fabric of photochemical catalyst coating |
| CN101705613B (en) * | 2009-11-03 | 2011-12-14 | 东华大学 | Method for preparing flexible air purifying material by low temperature in situ synthesis |
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