CN101775743B - Method for preparing Ag modified TiO2 composite air purifying function fabric in situ at low temperature - Google Patents
Method for preparing Ag modified TiO2 composite air purifying function fabric in situ at low temperature Download PDFInfo
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- CN101775743B CN101775743B CN2009102002208A CN200910200220A CN101775743B CN 101775743 B CN101775743 B CN 101775743B CN 2009102002208 A CN2009102002208 A CN 2009102002208A CN 200910200220 A CN200910200220 A CN 200910200220A CN 101775743 B CN101775743 B CN 101775743B
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Abstract
The invention relates to a method for preparing an Ag modified TiO2 composite air purifying function fabric in situ at low temperature, which comprises the following steps of: (1) ultrasonically washing a fabric by an acetone solution, drying and processing in an efficient cleaning agent; (2) soaking and rolling the fabric in an antioxidant finishing solution LZQ, pre-baking and baking at 130-150 DEG C; (3) adding titanium (IV) isopropoxide into anhydrous alcohol in an inert environment and adding a stabilizing agent, a mixed solution of anhydrous alcohol, acid and deionized water and a wetting agent; (4) soaking the fabric into sol, drying, removing the sol retained on the surface of a material and drying again; and (5) processing the dried fabric in boiling water, prebaking at 40-50 DEG C again, soaking in a silver nitrate solution and obtaining the composite air purifying fabric by the irradiation of a quasi-molecule ultraviolet light source. The invention has simple method, low cost and no secondary pollution and is easy for industrialized production, and the obtained flexible air purifying material has good air purifying effect.
Description
Technical field
The invention belongs to the preparation field of composite air purifying function fabric, particularly relate to a kind of low temperature in-situ growth Ag and modify TiO
2The method of composite air purifying function fabric.
Background technology
In recent years, along with the fast development of China's economy and the raising day by day of people's lives, the finishing level in office and inhabitation place is more and more higher, and emerging construction material particularly chemical synthesis building materials is widely used in top-grade furniture, household electrical appliance, enters family and office one after another.Spices, cosmetics, glazing agent, air freshener, insect-proof agent, pesticide, washing agent etc. have also become requisite articles for use in people's life.People are when enjoying comfortable and satisfied that these products bring, and they are just constantly producing all contaminations matter and harmful substance, and the destruction IAQ (indoorairquality, IAQ).And building energy conservation, indoor heat insulating, unified air-conditioning etc. make the better tightness of room and office space, and the pollutant of indoor generation is difficult to cause the deterioration of IAQ to outdoor diffusion.These factors have caused all no matter harmful substance constantly increases in the room air on kind or quantitatively, thereby have produced room air pollution.
Studying data at home and abroad in recent years shows, the city dweller has time of 80% to spend in various indoor environments every day approximately, and responsive crowds such as old man and children are longer in the indoor time of spending, thereby the indoor air quality is very important to health effects.Live in for a long time people in such building can occur headache, respiratory tract infection, tired drowsiness, heating is felt sick, the skin convulsion is itched and symptom such as abnormality allergy, these syndromes be collectively referred to as " ill building syndrome " (sickbuilding syndrome, SBS).Room air pollution has been listed in one of five big factors that are detrimental to health in the world, and is of common occurrence about the report that indoor pollution causes health to be endangered.Only one to just finding to have 16% people to suffer from the mucosal inflammation relevant with work (, nose or throat inflammation) in 2060 people's the random experiments, and 7% people is indoor, especially suffers from these diseases in office.Operating efficiency decline, employee's sick leave and direct medical cost etc. that indoor air quality decline causes have caused a large amount of economic losses.According to detection data to China's part building room air pollution level, newly fit up the serious room of after stain, the peak concentration of formaldehyde in indoor air can reach 0.8～1mg/m
3, surpass national standard limit value (0.08mg/m
3) more than 10 times, indivedual even up to 0.8～1mg/m
3Have document to show, indoorly detect more than 300 kind of pollutant, the indoor air level of pollution generally will exceed 2-5 doubly than outdoor environment, under the extreme case, and can be above 100 times.Abominable room air brings serious harm to human beings'health.City dweller about 80% time is spent indoor, and being in the potential hazard that is suffered in the abominable indoor environment for a long time can't estimate.Along with the enhancing of health of people consciousness and sense of self-protection, more and more higher to the requirement of quality of life and indoor environment, begin to recognize that the quality that improves room air is the guarantee of healthy living and work.Past people's notice is placed on the air pollution of outdoor environment always and administers, but the nearly more than ten years, IAQ also becomes the problem that the whole world generally is concerned about day by day to the human body health affected.
Therefore, administer room air pollution and especially remove the focus that organic pollution in the room air becomes domestic and international scientific worker's research.At present, the method for removal indoor air pollutants mainly contains: physisorphtion, chemical neutralisation, photocatalytic method, negative aeroion method etc.But above method exist absorption saturated, make complicated, cost is high and defective such as the use of can not regenerating.Consider that flexible parent metal (fibrous material) has big, the easy machine-shaping of surface area, enrichment pollutant and dilution catabolite property as carrier, photochemical catalyst is loaded to prepare flexible air purifying material on the flexible parent metal.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.Because the flexible parent metal non-refractory has limited photochemical catalyst and has deposited on flexible parent metal, carries out the use of crystal formation conversion method again.
Summary of the invention
Technical problem to be solved by this invention provides a kind of low temperature in-situ growth Ag and modifies TiO
2The method of composite air purifying function fabric, this method is simple, cost is low, and non-secondary pollution is easy to suitability for industrialized production; The flexible air purifying material good air purification effect of gained.
A kind of low temperature in-situ growth Ag of the present invention modifies TiO
2The method of composite air purifying function fabric comprises:
(1) preliminary treatment
With acetone soln ultrasonic cleaning fabric 30～50min, 20～30 ℃ of dryings 12～16 hours, again in efficient cleaner Kieralon OL (BASF AG) solution 40～45 ℃ handled 80～85 ℃ of drying 30～45min 20～30 minutes down;
(2) fabric anti-photooxidation protection arrangement
Take out after pretreated fabric padded anti-oxidant finisher solution LZQ 30～50min,, be warming up to 130～150 ℃ again and bake 2～4min at 70～80 ℃ of preliminary dryings; Wherein LZQ dressing liquid composition is, 1～3% Tween 80,4～10% nanometer hydroxyapatite MP40,3～8% four seasons Doutrates, 6～10% octyl group trimethoxy silanes and 69～86% water are formed;
(3) under inert environments, under stirring action, slowly join 0.02～0.15mol titanium tetraisopropylate in 30～50ml absolute alcohol, add 0.01～0.03mol stabilizing agent again, 200～300rpm stirs 1～4min, continuation adding 20～100ml volume ratio is 30: 1: 5～60: 1: 1.5 absolute alcohol, acid and a deionized water mixed liquor then, stir 40～100min, add wetting agent, obtain the low temperature precursor sol;
(4) the fabric face original position is synthetic
To arrive 3～10min in step (3) colloidal sol through the textile impregnation that step (2) is handled, 65～70 ℃ of oven dry down, remove the residual colloidal sol of material surface afterwards, dry 3～8min down at 90～95 ℃ then;
(5) post processing
Fabric after the oven dry was handled 2～4 hours in 90～100 ℃ of boiling water, again at 40～50 ℃ of preliminary dryings, be immersed in 1～3min in 0.001～0.01mol/L liquor argenti nitratis ophthalmicus then, irradiation 3～6 minutes under quasi-molecule ultraviolet source obtains the compound air purification fabric then.
The fabric of described step (1) is non-weaving cloth, woven cloth or knitted cloth.
The fiber of described fabric is selected from cotton fiber, flax fibre, polyimide fiber, activated carbon fiber, polyester fiber, polypropylene fibre, bamboo fibre, one or both blend fibres in silk fiber, wool fibre, soybean fiber, milk protein fiber, the nylon fibre.
Alcohol in the described step (3) is isopropyl alcohol, isobutanol or isoamyl glycol.
Acid in the described step (3) is hydrochloric acid, nitric acid, sulfuric acid or acetic acid.
Wetting agent in the described step (3) is Tween 80 or Qu Latong 100, and consumption is: owf 2%～6%.
Stabilizing agent in the described step (3) is triethylamine or triethanolamine; Acid is hydrochloric acid, nitric acid, sulfuric acid or acetic acid.
Radiation parameter in the described step (5): wavelength 222 or 172nm, frequency 100Hz, electric current 1.6A, power 1.5KW, fluorescent tube is 1～3cm with the space of handling fabric.
The material for air purification of the present invention's preparation can be applicable to interior decoration fields such as submarine, hospital ward, automotive interior trim, interior of aircraft decoration, has broad application prospects and market prospects.
The present invention is directly by arrangement anti-photooxidation protective layer on fabric, and the synthetic photochemical catalyst of original position on fabric is realized the conversion of photochemical catalyst crystal formation in boiling water then, the synthetic flexible air purifying material of preparation low-temperature in-site.
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) the fibrous raw material source is wide, easily is processed into different shape, and is easy to use;
(3) the present invention on fabric, had both solved the dust pollution question of photochemical catalyst when air cleaning with the semi-conductor nano particles growth in situ, can avoid the problem of photochemical catalyst reunion decrease in efficiency on flexible parent metal again; The photo-catalyst film on flexible air 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 photocatalytic degradation toxic gas under visible light, and it is become nonpoisonous and tasteless material, flexible air purifying material good air purification 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 to the present invention is described 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 30min, 20 ℃ of room temperatures dry 12 hours down, again in the efficient cleaner Kieralon of BASF AG OL solution 40 ℃ handled 20 minutes 80 ℃ of dry 30min down down;
(2) wool fabric anti-photooxidation protection arrangement
Take out after wool fabric padded the anti-oxidant dressing liquid LZQ of fiber 30min,, be warming up to 130 ℃ again and bake 2min at 70 ℃ of preliminary dryings; Wherein LZQ dressing liquid composition is, 1～3% Tween 80,4～10% nanometer hydroxyapatite MP, 40,3～8% four seasons Doutrates, 6～10% octyl group trimethoxy silanes and 69～86% water are formed;
(3) preparation of low temperature presoma
Under inert environments, under stirring action, slowly join the 0.02mol titanium tetraisopropylate in the 30mL isopropyl alcohol, the 0.01mol triethylamine is joined in the mixed liquor as stabilizing agent, stir 1min at 200rpm, continue adding 20mL then, to contain volume ratio be 30: 1: 5 isopropyl alcohol, hydrochloric acid, deionized water mixed solution, stir 40min, add relative fabric and weigh 2% wetting agent Tween 80, obtain the low temperature precursor sol.
(4) the wool fabric surface in situ is synthetic
Wool fabric is impregnated into 3min in the above-mentioned colloidal sol, the flexible material behind the dipping 65 ℃ of oven dry down, is removed the residual colloidal sol of material surface, then oven dry 3min under 90 ℃.
(5) post processing of composite air purifying function fabric
Boiled 2 hours in the compound air purification fabric boiling water with step (4) preparation, the sample that boiling water treating is crossed is at 40 ℃ of preliminary dryings, be immersed in 1min in the 0.001mol/L liquor argenti nitratis ophthalmicus then, being placed on apart from the wavelength of fluorescent tube 1cm then is irradiation 3 minutes under the 222nm quasi-molecule ultraviolet source, obtains the compound air purification fabric.
Composite air purifying function fabric and common activated carbon air purifying material that the present invention is made are respectively charged in the air purifier of same model, and under identical conditions: comprise the space, harmful gas concentration, time compare test, and its result is as follows:
Embodiment 2
(1) surface of cotton fabric preliminary treatment
With acetone soln ultrasonic cleaning COTTON FABRIC 40min, 25 ℃ of room temperatures dry 14 hours down, again in efficient cleaner Kieralon OL solution 43 ℃ handled 25 minutes 83 ℃ of dry 37min down down;
(2) COTTON FABRIC anti-photooxidation protection arrangement
Take out after COTTON FABRIC padded the anti-oxidant dressing liquid LZQ of fiber 40min,, be warming up to 140 ℃ again and bake 3min at 75 ℃ of preliminary dryings; Wherein LZQ dressing liquid composition is, 1～3% Tween 80,4～10% nanometer hydroxyapatite MP40,3～8% four seasons Doutrates, 6～10% octyl group trimethoxy silanes and 69～86% water are formed.
(3) preparation of low temperature presoma
Under inert environments, under stirring action, slowly join the 0.08mol titanium tetraisopropylate in the 40mL isobutanol, the 0.02mol triethylamine is joined in the mixed liquor as stabilizing agent, stir 2min at 250rpm, continuation adding 60mL volume ratio is 45: 1: 2 isopropyl alcohol, nitric acid, a deionized water mixed solution then, stir 70min, add relative fabric and weigh 4% wetting agent Tween 80, obtain the low temperature precursor sol.
(4) the surface of cotton fabric original position is synthetic
COTTON FABRIC is impregnated into 7min in the above-mentioned colloidal sol, the flexible material behind the dipping 67 ℃ of oven dry down, is removed the residual colloidal sol of material surface, then oven dry 5min under 93 ℃.
(5) post processing of composite air purifying function fabric
Boiled 2 hours in the compound air purification fabric boiling water with step (4) preparation, the sample that boiling water treating is crossed is at 45 ℃ of preliminary dryings, be immersed in 3min in the 0.005mol/L liquor argenti nitratis ophthalmicus then, being placed on apart from the wavelength of fluorescent tube 2cm then is irradiation 4 minutes under the 222nm quasi-molecule ultraviolet source, obtains the compound air purification fabric.
Composite air purifying function fabric and common activated carbon air purifying material that the present invention is made are respectively charged in the air purifier of same model, and under identical conditions: comprise the space, harmful gas concentration, time compare test, and its result is as follows:
Embodiment 3
(1) sodolin surface preparation
With acetone soln ultrasonic cleaning COTTON FABRIC 50min, 30 ℃ of room temperatures dry 16 hours down, again in efficient cleaner Kieralon OL solution 45 ℃ handled 30 minutes 85 ℃ of dry 45min down down;
(2) sodolin anti-photooxidation protection arrangement
Take out after sodolin padded the anti-oxidant dressing liquid LZQ of fiber 50min,, be warming up to 150 ℃ again and bake 4min at 80 ℃ of preliminary dryings; Wherein LZQ dressing liquid composition is, 1～3% Tween 80,4～10% nanometer hydroxyapatite MP40,3～8% four seasons Doutrates, 6～10% octyl group trimethoxy silanes and 69～86% water are formed.
(3) preparation of low temperature presoma
Under inert environments, under stirring action, slowly join the 0.15mol titanium tetraisopropylate in the 50mL isobutanol, the 0.03mol triethylamine is joined in the mixed liquor as stabilizing agent, stir 4min at 300rpm, continue to add 60: 1: 1.5 isopropyl alcohol of 100mL volume ratio, acetic acid, deionized water mixed solution then, stir 100min, add relative fabric and weigh 6% wetting agent Tween 80, obtain the low temperature precursor sol.
(4) the sodolin surface in situ is synthetic
COTTON FABRIC is impregnated into 10min in the above-mentioned colloidal sol, the flexible material behind the dipping 70 ℃ of oven dry down, is removed the residual colloidal sol of material surface, then oven dry 8min under 95 ℃.
(5) post processing of composite air purifying function fabric
Boiled 2 hours in the compound air purification fabric boiling water with step (4) preparation, the sample that boiling water treating is crossed is at 50 ℃ of preliminary dryings, be immersed in 3min in the 0.01mol/L liquor argenti nitratis ophthalmicus then, being placed on apart from the wavelength of fluorescent tube 2cm then is irradiation 4 minutes under the 222nm quasi-molecule ultraviolet source, obtains the compound air purification fabric.
Air self-purifying function fabric and common activated carbon air purifying material that the present invention is made are respectively charged in the air purifier of same model, and under identical conditions: comprise the space, harmful gas concentration, time compare test, and its result is as follows:
Claims (8)
1. a low temperature in-situ growth Ag modifies TiO
2The method of composite air purifying function fabric comprises:
(1) preliminary treatment is with acetone soln ultrasonic cleaning fabric 30～50min, 20～30 ℃ of dryings 12～16 hours, again in efficient cleaner Kieralon OL solution 40～45 ℃ handled 80～85 ℃ of drying 30～45min 20～30 minutes down;
(2) take out after pretreated fabric being padded anti-oxidant finisher solution LZQ 30～50min,, be warming up to 130～150 ℃ again and bake 2～4min at 70～80 ℃ of preliminary dryings; Wherein LZQ dressing liquid composition is, 1～3% tween, 4～10% nanometer hydroxyapatites, 3～8% four seasons Doutrates, 6～10% octyl group trimethoxy silanes and 69～86% water are formed;
(3) under inert environments, under stirring action, slowly join 0.02～0.15mol titanium tetraisopropylate in 30～50ml absolute alcohol, add 0.01～0.03mol stabilizing agent again, 200～300rpm stirs 1～4min, continuation adding 20～100ml volume ratio is 30: 1: 5～60: 1: 1.5 absolute alcohol, acid and a deionized water mixed liquor then, stir 40～100min, add wetting agent, obtain the low temperature precursor sol;
(4) will arrive 3～10min in step (3) colloidal sol through the textile impregnation that step (2) is handled, 65～70 ℃ of oven dry down, remove the residual colloidal sol of material surface afterwards, dry 3～8min down at 90～95 ℃ then;
(5) fabric after the oven dry was handled 2～4 hours in 90～100 ℃ of boiling water, again at 40～50 ℃ of preliminary dryings, be immersed in 1～3min in 0.001～0.01mol/L liquor argenti nitratis ophthalmicus then, irradiation 3～6 minutes under quasi-molecule ultraviolet source obtains the compound air purification fabric then.
2. a kind of low temperature in-situ growth Ag according to claim 1 modifies TiO
2The method of composite air purifying function fabric is characterized in that: the fabric of described step (1) is non-weaving cloth, woven cloth or knitted cloth.
3. a kind of low temperature in-situ growth Ag according to claim 2 modifies TiO
2The method of composite air purifying function fabric, it is characterized in that: the fiber of described fabric is selected from cotton fiber, flax fibre, polyimide fiber, activated carbon fiber, polyester fiber, polypropylene fibre, bamboo fibre, one or both blend fibres in silk fiber, wool fibre, soybean fiber, milk protein fiber, the nylon fibre.
4. a kind of low temperature in-situ growth Ag according to claim 1 modifies TiO
2The method of composite air purifying function fabric is characterized in that: the alcohol in the described step (3) is isopropyl alcohol, isobutanol or isoamyl glycol.
5. a kind of low temperature in-situ growth Ag according to claim 1 modifies TiO
2The method of composite air purifying function fabric is characterized in that: the acid in the described step (3) is hydrochloric acid, nitric acid, sulfuric acid or acetic acid.
6. a kind of low temperature in-situ growth Ag according to claim 1 modifies TiO
2The method of composite air purifying function fabric is characterized in that: the wetting agent in the described step (3) is tween or Qu Latong, and consumption is: owf 2%～6%.
7. a kind of low temperature in-situ growth Ag according to claim 1 modifies TiO
2The method of composite air purifying function fabric is characterized in that: the stabilizing agent in the described step (3) is triethylamine or triethanolamine.
8. a kind of low temperature in-situ growth Ag according to claim 1 modifies TiO
2The method of composite air purifying function fabric is characterized in that: the radiation parameter in the described step (5): wavelength 222 or 172nm, and frequency 100Hz, electric current 1.6A, power 1.5KW, fluorescent tube is 1～3cm with the space of handling fabric.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009102002208A CN101775743B (en) | 2009-12-10 | 2009-12-10 | Method for preparing Ag modified TiO2 composite air purifying function fabric in situ at low temperature |
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|---|---|---|---|
| CN2009102002208A CN101775743B (en) | 2009-12-10 | 2009-12-10 | Method for preparing Ag modified TiO2 composite air purifying function fabric in situ at low temperature |
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| CN101775743B true CN101775743B (en) | 2011-08-31 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102634977B (en) * | 2012-04-24 | 2013-06-05 | 南通大学 | Method for preparing anti-bacterial fibers and fabrics by in-situ complexometry |
| CN103031707A (en) * | 2012-12-27 | 2013-04-10 | 德清诺普医药科技有限公司 | Deodorant, antibacterial and anti-fouling complexing agent for fabric |
| CN103061108A (en) * | 2012-12-27 | 2013-04-24 | 德清诺普医药科技有限公司 | Method for smell removal, disinfection and stain resistance process on fabric |
| CN103205889B (en) * | 2013-04-17 | 2014-11-05 | 东华大学 | Preparation method of visible photocatalytic functional fabric in interface nanometer mixed crystal structure |
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| CN1257461A (en) * | 1997-05-23 | 2000-06-21 | 株式会社京绒 | Titanium oxide-containing material and process for preparing the same |
| CN1792437A (en) * | 2005-12-02 | 2006-06-28 | 厦门大学 | Method for loading silver nanometer particles onto nanometer titanium dioxide |
| US20060141015A1 (en) * | 2004-12-07 | 2006-06-29 | Centre Des Technologies Textiles | Antimicrobial material |
| CN1936168A (en) * | 2006-08-08 | 2007-03-28 | 中原工学院 | Fabric product finishing agent and its preparing process and method thereof |
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2009
- 2009-12-10 CN CN2009102002208A patent/CN101775743B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257461A (en) * | 1997-05-23 | 2000-06-21 | 株式会社京绒 | Titanium oxide-containing material and process for preparing the same |
| US20060141015A1 (en) * | 2004-12-07 | 2006-06-29 | Centre Des Technologies Textiles | Antimicrobial material |
| CN1792437A (en) * | 2005-12-02 | 2006-06-28 | 厦门大学 | Method for loading silver nanometer particles onto nanometer titanium dioxide |
| CN1936168A (en) * | 2006-08-08 | 2007-03-28 | 中原工学院 | Fabric product finishing agent and its preparing process and method thereof |
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