CN1724143A - Process for preparing photocatalyst composite material - Google Patents
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- CN1724143A CN1724143A CN 200410028196 CN200410028196A CN1724143A CN 1724143 A CN1724143 A CN 1724143A CN 200410028196 CN200410028196 CN 200410028196 CN 200410028196 A CN200410028196 A CN 200410028196A CN 1724143 A CN1724143 A CN 1724143A
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Abstract
A composite photo-catalyst for cleaning air and treating drinking water and sewage is prepared from foam metal or metallic net through electrochemical anodizing to its surface, flash plating in the low-concentration aqueous solution containing Cu and RE to form binding layer and diffusing layer, electrophoresis in the organo-titanium sol with photo-catalytic activity, drying in air and low-temp sintering. It has high specific surface area, photo-catalytic activity and antibacterial performance.
Description
Technical field:
The present invention relates to a kind of preparation method of photocatalyst composite, particularly foam metal or tiltedly lashing wire belong to the preparation method of the photocatalyst composite of online composite Nano catalysis material.Belong to the nano surface work field.
Background technology:
Photocatalysis technology is the most promising air that at home and abroad gains public acceptance at present, the optimal technology of water treatment.Research to relevant composition in the catalysis material can be traced back to 19th-century.But, just really find the using value that it is huge fields such as healthy and environmental protection Japan scientist until nineteen nineties.Over nearly 5 years, Japan utilizes catalysis material to formulate miscellaneous application product in weaving, drinking water treatment, cosmetics, food, medicine and air purification field etc., and its annual value of production has reached 20,000,000,000 dollars in calendar year 2001.Therefore, this material is described as 21st century illusion material; The Nature is vouchsafed the mankind's rarity etc.Following closely, sharply intensification is used also to the research and the market of catalysis material in Korea S, the U.S. and Taiwan etc.
In recent years, the progress of nano material process technology makes with the nano titanium oxide to be that the catalysis material of representative has obtained extensive research, because titanium dioxide (TiO
2) the photocatalysis antibacterial material action effect is lasting, utilize the ultraviolet light that contains in sunshine, the fluorescent lamp to make excitaton source and just can have antimicrobial effect, and have purify air, photocatalytic effect such as sewage disposal, automatically cleaning, aspect environmental protection, show application prospects, become the inorganic antibacterial scavenging material of a new generation.Nano-TiO through doping treatment and finishing
2Photocatalytic product, technical matters is simple, with low cost in actual applications, utilize natural daylight to get final product catalytic decomposition bacterium and pollutant, have advantages such as high catalytic activity, good chemical stability and heat endurance, non-secondary pollution, nonirritant, safety non-toxic, and can be of value to the ecological natural environment for a long time, be one of environmental protection catalyst that has most DEVELOPMENT PROSPECT.
But, the dispersion of nano-photocatalyst material and to support be major issue in using, the suitable work particle diameter of nano-photocatalyst material is 30～50 nanometers, disperses extremely difficulty to accomplish with the finished product powder, has a strong impact on operating efficiency.Seeking suitable supporting material and support way, also is can decision obtain practical application in air, water treatment field key, and the product that can see on the market is divided into:
1. direct application type: the photocatalyst powder is mixed with binding agent, coat on the porous materials such as sponge, honeycomb cardboard, because nano material not by fine dispersion, adds the masking action of binding agent, the photocatalysis effect is faint.
2. titanium sol impregnation type: the titanium colloidal sol that forms with the titanate ester hydrolysis is presoma, temperature-resistant materials such as glass fibre, woven wire is flooded lift, and carries out sintering with the temperature about 500 degree again, finishes the crystalline form conversion.This mode response area is little, photocatalysis efficiency is low.
3. composite electrodeposition photocatalysis powder material on the foam metal nickel material: titanium dioxide powder is extremely difficult to be disperseed in ion type liquid and keeps, and the particle of reunion has not been a nano material; Surface coverage is low excessively, is no more than 70%, and photocatalytic activity is lower.
Find that through the file retrieval publication number is the Chinese invention patent of CN1486785A, denomination of invention is " preparation method of foam metal load TiO2 nano-photo catalytic screen pack ".This patent disclosure a kind of be the photocatalysis filter screen that carrier carries out load with the foam metal, at first foam metal is carried out oxidation processes, in the colloidal sol that with titanate ester or titanium tetrachloride is presoma, flood drying, sintering and make again.This method needs twice sintering, the fibre wall of foam metal as thin as a wafer, oxidation and sintering process can have a strong impact on the intensity and the pliability of foam metal, the product of making is crisp, bad mechanical strength is unfavorable for using, simultaneously the product activity under visible light not.
Summary of the invention:
The objective of the invention is to make a kind of preparation method who is suitable for the required efficiency light catalyst composite of present air cleaning, purification of water quality.
The technical solution adopted in the present invention is: at first,, electrochemical anodic oxidation is carried out on its surface handle as matrix with foam metal or wire netting, make its surface form the crystalline state nanometer structure of bigger serface; Secondly, will form binder course and diffusion layer through matrix compound flash in containing the low concentration Watts bath of copper and rare earth element of above-mentioned processing; Then, will in the organic titanium colloidal sol that has configured, carry out the electrophoresis dipping through the matrix of flash with photocatalytic activity, air-dry after taking out; At last, place the low-temperature sintering stove to carry out sintering the matrix after air-dry, obtain the photocatalyst composite.
Described foam metal is a kind of in foam metal nickel, foam metal copper, the foam metal iron; The described wire netting that tiltedly draws is a kind of in nickel, copper, the iron, and its thickness is less than 0.1 millimeter, and the aperture is less than 1 millimeter.
Electrochemical anodic oxidation is carried out on described surface, and to handle the electrolyte adopted be the sulfuric acid of 0.3～2 molar concentration, and negative electrode uses corrosion resistant plate.
Described in containing the low concentration Watts bath of copper and rare earth element compound flash, a watt electroplate liquid formulation whenever is upgraded to nickelous sulfate 70～110 gram, nickel chloride 30～80 grams, boric acid 30～40 grams, iron chloride 5～10 grams, rare earth chloride 0.5～2 gram, ATPN0.01～0.5 gram.
It is the presoma configuration that described organic titanium colloidal sol with photocatalytic activity adopts tetrabutyl titanate, and the concrete configuration method is:
(1), calculates with weight ratio, prepare 3%～30% tetrabutyl titanate, 60%～90% absolute ethyl alcohol, the sulfuric acid of 0.5%～2% hydrochloric acid or 40% concentration, 3%～5% ethyl orthosilicate, 0.1%～0.5% the copper sulphate and the mixed solution of rare earth chloride, 0.5%～2% nano-titanium dioxide powder;
(2), tetrabutyl titanate is joined in the ethanol under stirring, under high-speed stirred, splash into hydrochloric acid or sulfuric acid then;
(3), the mixed liquor that under stirring, adds copper sulphate and rare earth chloride;
(4), under stirring, with ultraviolet lamp irradiation, 2～50 hours time;
(5), under stirring, drip ethyl orthosilicate;
(6), under stirring, will be through adding, and continuous stirring 1～3 hour with the auxiliary nano titanium dioxide powder that soaks into of ethanol and ultrasonic wave;
The organic titanium colloidal sol with photocatalytic activity that (7), will prepare leaves standstill and got final product in 24 hours.
Adopt the composite photo catalyst material of made of the present invention, have the following advantages:
1. Biao Mian microstructure can produce attached collection effect to pernicious gas, is easy to form the photocatalysis basic effect of " absorption-mass transfer-reaction ", guarantees carrying out normally and efficiently of light-catalyzed reaction;
2. big specific area and photocatalyst material are in nanoscale, and compound catalysis material response area is increased, and middle composite deposite makes the required excitation source red shift of photocatalyst work, and the efficiency of light energy utilization increases, and improves quantum efficiency, strengthens the catalytic action effect;
3. can resist the structural deterioration effect of the strong oxidizer of photocatalytic process middle-ultraviolet lamp and generation, can be designed to standarized component and use for a long time;
4. be convenient to improve free radical quantum reaction efficiency by the mode of externally-applied magnetic field, electric field;
5. be easy to machine-shaping, the surface is capable of washing.
The specific embodiment:
The present invention is with foam metal or tiltedly draws wire netting is matrix, at first electrochemical anodic oxidation being carried out on its surface handles, make the surface form the crystalline state nanometer structure of bigger serface, compound flash in containing the low concentration Watts bath of iron and rare earth element again, in the organic titanium colloidal sol that has configured, carry out the electrophoresis dipping then with photocatalytic activity, take out the back natural air drying, place the low-temperature sintering stove to carry out sintering, carry out low sintering temperature and be generally 150～300 degree.Make efficiency light catalyst composite at last, the product photocatalyst activity composition of making accounts for 4～10% of product gross weight.
Wherein, foam metal is a kind of in foam metal nickel, foam metal copper, the foam metal iron; The described wire netting that tiltedly draws is a kind of in nickel, copper, the iron, and thickness is less than 0.1 millimeter, and the aperture is less than 1 millimeter.It is more firm for photocatalysis layer is combined with it, specific area is bigger, activity is higher, at first anodized is carried out on its surface, the electrolyte that adopts is the sulfuric acid of 0.3～2 molar concentration, and negative electrode uses corrosion resistant plate, electric current 1～5A, 1～30 minute time, composite deposition flash in containing the low concentration Watts bath of copper and rare earth element then, a watt electroplate liquid formulation whenever is upgraded to: nickelous sulfate 70～110 grams, nickel chloride 30～80 grams, boric acid 30～40 grams, iron chloride 5～10 grams, rare earth chloride 0.5～2 gram, ATPN0.01～0.5 gram, current density 2～15A, 3～60 seconds time.Through described two step pretreated foam metals or tiltedly draw wire netting, the surface forms the nanometer crystal structure, and composite electrodeposition one deck intermediate layer combines firmly with catalysis material simultaneously, and specific area is big, the photocatalytic activity height.
In the said process, the organic titanium colloidal sol employing tetrabutyl titanate with photocatalytic activity is the presoma configuration, and the concrete configuration method is:
(1), calculates with weight ratio, prepare 3%～30% tetrabutyl titanate, 60%～90% absolute ethyl alcohol, the sulfuric acid of 0.5%～2% hydrochloric acid or 40% concentration, 3%～5% ethyl orthosilicate, 0.1%～0.5% the copper sulphate and the mixed solution of rare earth chloride, 0.5%～2% nano-titanium dioxide powder;
(2), tetrabutyl titanate is joined in the ethanol under stirring, under high-speed stirred, splash into hydrochloric acid or sulfuric acid then;
(3), the mixed liquor that under stirring, adds copper sulphate and rare earth chloride;
(4), under stirring, with ultraviolet lamp irradiation, 2～50 hours time;
(5), under stirring, drip ethyl orthosilicate;
(6), under stirring, will be through adding, and continuous stirring 1～3 hour with the auxiliary nano titanium dioxide powder that soaks into of ethanol and ultrasonic wave;
The organic titanium colloidal sol with photocatalytic activity that (7), will prepare leaves standstill and got final product in 24. hours.
In conjunction with content of the present invention, provide following examples:
Embodiment 1:
One. have the organic titanium colloidal sol configuration of photocatalytic activity.
(1) weighing tetrabutyl titanate 200g, absolute ethyl alcohol 735 grams, sulfuric acid 10 grams of 37% hydrochloric acid or 40% concentration, ethyl orthosilicate 40 grams, mixed solution 5 grams of copper sulphate and rare earth chloride, nano-titanium dioxide powder 10 grams;
(2) tetrabutyl titanate is joined in the ethanol under stirring, under high-speed stirred, splash into hydrochloric acid or sulfuric acid then;
(3) stirring adds the mixed liquor of copper sulphate and rare earth chloride down;
(4) under the stirring, with ultraviolet lamp irradiation, 20 hours time;
(5) under the stirring, drip ethyl orthosilicate;
(6) under the stirring, will be through adding with the auxiliary nano titanium dioxide powder that soaks into of ethanol and ultrasonic wave, and continuous stirring 1～3 hour;
The organic titanium colloidal sol with photocatalytic activity that (7) will prepare left standstill 24 hours, and ageing is standby.
Two, the sulfuric acid solution of configuration 1Mol concentration is as anodic oxidation electrolyte.
Three, configuration composite deposition flash electrolyte, press every liter of addition weighing: nickelous sulfate 90 grams, nickel chloride 50 grams, boric acid 30 grams, frerrous chloride 7 grams, rare earth chloride 1 restrains, the ATPN0.02 gram.Announce that by electroplating handbook known watt electrolyte dosing mode is configured, wherein ATPN is earlier with adding behind a small amount of diluted hydrochloric acid dissolution.
Four, select finished foam metallic nickel (70PPI, surface density 300 grams, 2.5 millimeters of thickness for use, Shenzhen is melted the emerging battery material of connection Co., Ltd and is produced, and PPI refers to the per inch number of pores), at first in surperficial anodic oxidation electrolytic cell, carry out electrolytic treatments, select electric current 2.5A for use, 12 minutes time; Take out the dried raffinate of back control, directly put into the electronickelling of composite deposition groove, iron, rare earth alloy, electric current 10A, electroplating time 10 seconds takes out the after washing oven dry.
Five, surface treated foam metal oven dry back being impregnated in the organic titanium colloidal sol with photocatalytic activity at once, is anode with the titanium plate, applies 70 volts of DC voltages, carries out electrophoretic deposition, and 3 minutes time, the centre is stirred the discharge bubble gently.
Six, with the foam metal air dry of impregnation process 1 hour, put into baking oven, bake out temperature 150 degree, 10 minutes time.
Seven, repeat 5～6 steps 1 time.Form the photocatalysis nano material film on the foam metal surface, wherein the titanium dichloride load amount is 7.5%.
Eight, get the high efficiency photocatalysis composite of 300X300 millimeter area, put into 1 cubic metre of test box, 100 millimeters uviol lamps of placing 8 watts of distance, the another side distance is placed an instrument fan for 200 millimeters.Inject 1 milligram of formaldehyde with micropipette, opened fan 15 minutes, make inner concentration reach balance, open uviol lamp, use the multi-parameter on-line detector (to measure ammonia simultaneously, organic volatile sum total (TVoc), carbon dioxide, humidity, temperature, model IAQRAE-PGM5210), formaldehyde tester (model ppm FormaldemeterTM 400) carries out follow-on test, 0.83 milligram/cubic metre of initial concentration of formaldehyde, gas concentration lwevel 1020ppm, after 15 minutes, concentration of formaldehyde is reduced to 0.15 milligram, and gas concentration lwevel rises to 1205ppm, the Degradation Formaldehyde rate is 82%, course of reaction meets first-order kinetics equation (Lang Miuer-Xie Xiaer Wood equation is called for short the L-H equation) through The Fitting Calculation.
Embodiment 2:
By requirement configuration titanium colloidal sol among the embodiment 1, composite electrodeposition liquid, anodic oxidation electrolyte concentration 0.5Mol.
One, selects semi-finished product foam metal nickel (70PPI, surface density 90 grams, 2.5 millimeters of thickness for use, Shenzhen is melted the Co., Ltd's production of the emerging battery material of connection or is used the known technology self-control), at first in surperficial anodic oxidation electrolytic cell, carry out electrolytic treatments, select electric current 1.5A for use, 6 minutes time; Take out the dried raffinate of back control, directly put into the electronickelling of composite deposition groove, iron, rare earth alloy, electric current 10A, electroplating time 15 seconds takes out the after washing oven dry.
Two, surface treated foam metal oven dry back being impregnated in the organic titanium colloidal sol with photocatalytic activity at once, is anode with the titanium plate, applies 90 volts of DC voltages, carries out electrophoretic deposition, and 2 minutes time, the centre is stirred the discharge bubble gently.
Three, with the foam metal air dry of impregnation process 1 hour, put into baking oven, bake out temperature 130 degree, 5 minutes time.
Four, repeat the second～three step 1 time.Form the photocatalysis nano material film on the foam metal surface, wherein the titanium dichloride load amount is 4.7%.
Five, get the high efficiency photocatalysis composite of 300X300 millimeter area, put into 1 cubic metre of test box, distance is placed 8 watts of uviol lamps for 100 millimeters, and the another side distance is placed an instrument fan for 200 millimeters.Inject 1 milligram of formaldehyde with micropipette, opened fan 15 minutes, make inner concentration reach balance, open uviol lamp, use the multi-parameter on-line detector, the formaldehyde tester carries out follow-on test, 0.85 milligram/cubic metre of initial concentration of formaldehyde, gas concentration lwevel 1060ppm, after 15 minutes, concentration of formaldehyde is reduced to 0.13 milligram, gas concentration lwevel rises to 1285ppm, the Degradation Formaldehyde rate is 85%, and course of reaction meets the first-order kinetics equation through The Fitting Calculation.
Embodiment 3
By requirement configuration titanium colloidal sol among the embodiment 1, composite electrodeposition liquid, anodic oxidation electrolyte concentration 0.8Mol.
One, selects for use and tiltedly draw wire netting (0.05 millimeter of thickness, Shenzhen North Star non-ferrous metal company produce), at first in surperficial anodic oxidation electrolytic cell, carry out electrolytic treatments, select electric current 2A for use, 5 minutes time; Take out the dried raffinate of back control, directly put into the electronickelling of composite deposition groove, iron, rare earth alloy, electric current 4A, electroplating time 20 seconds takes out the after washing oven dry.
Two, surface treated foam metal oven dry back being impregnated in the organic titanium colloidal sol with photocatalytic activity at once, is anode with the titanium plate, applies 60 volts of DC voltages, carries out electrophoretic deposition, 3 minutes time.
Three, with the foam metal air dry of impregnation process 1 hour, put into baking oven, bake out temperature 180 degree, 2 minutes time.
Four, repeat 2～3 steps 1 time.Form the photocatalysis nano material film on the foam metal surface, wherein the titanium dichloride load amount is 5.7%.
Five, get three stacked the adding of high efficiency photocatalysis composite of 300 * 300 millimeters areas, put into 1 cubic metre of test box, distance is placed the 8W uviol lamp for 100 millimeters, and the another side distance is placed an instrument fan for 200 millimeters.Inject 1 milligram of formaldehyde with micropipette, opened fan 15 minutes, make inner concentration reach balance, open uviol lamp, use the multi-parameter on-line detector), the formaldehyde tester carries out follow-on test, 0.82 milligram/cubic metre of initial concentration of formaldehyde, gas concentration lwevel 1088ppm, after 15 minutes, concentration of formaldehyde is reduced to 0.16 milligram, gas concentration lwevel rises to 1264ppm, the Degradation Formaldehyde rate is 80%, and course of reaction meets the first-order kinetics equation through The Fitting Calculation.
The sample that embodiment 1 and embodiment 2 are made detects through the Guangdong Microbes Inst, under conditions such as unglazed, natural scattering light, fluorescent lamp, uviol lamp, the antibacterial effect of Escherichia coli, staphylococcus aureus is reached 99.99%.
Claims (7)
1, a kind of preparation method of photocatalyst composite, is characterized in that as matrix with foam metal or wire netting:
At first, matrix surface is carried out electrochemical anodic oxidation handle, make its surface form the crystalline state nanometer structure of bigger serface;
Secondly, will form binder course and diffusion layer through matrix compound flash in containing the low concentration Watts bath of copper and rare earth element of above-mentioned processing;
Then, will in the organic titanium colloidal sol that has configured, carry out the electrophoresis dipping through the matrix of flash with photocatalytic activity, air-dry after taking out;
At last, place the low-temperature sintering stove to carry out sintering the matrix after air-dry, obtain the photocatalyst composite.
2, the preparation method of a kind of photocatalyst composite according to claim 1 is characterized in that: described foam metal is a kind of in foam metal nickel, foam metal copper, the foam metal iron; The described wire netting that tiltedly draws is a kind of in nickel, copper, the iron, and its thickness is less than 0.1 millimeter, and the aperture is less than 1 millimeter.
3, the preparation method of a kind of photocatalyst composite according to claim 1 is characterized in that: electrochemical anodic oxidation is carried out on described surface, and to handle the electrolyte adopted be the sulfuric acid of 0.3～2 molar concentration, and negative electrode uses corrosion resistant plate.
4, the preparation method of a kind of photocatalyst composite according to claim 1, it is characterized in that: described in containing the low concentration Watts bath of iron and rare earth element compound flash, the watt electroplate liquid formulation whenever is upgraded to nickelous sulfate 70～110 grams, nickel chloride 30～80 grams, boric acid 30～40 grams, iron chloride 5～10 grams, rare earth chloride 0.5～2 gram, ATPN (carboxyethyl thiuronium) 0.01～0.5 gram.
5, the preparation method of a kind of photocatalyst composite according to claim 1 is characterized in that: it is the presoma configuration that described organic titanium colloidal sol with photocatalytic activity adopts tetrabutyl titanate, and the concrete configuration method is:
(1) calculates with weight ratio, prepare 3%～30% tetrabutyl titanate, 60%～90% absolute ethyl alcohol, the sulfuric acid of 0.5%～2% hydrochloric acid or 40% concentration, 3%～5% ethyl orthosilicate, the mixed solution of 0.1%～0.5% copper sulphate (or zinc sulfate) and rare earth chloride, 0.5%～2% nano-titanium dioxide powder;
(2) tetrabutyl titanate is joined in the ethanol under stirring, under high-speed stirred, splash into hydrochloric acid or sulfuric acid then;
(3) mixed liquor of adding copper sulphate and rare earth chloride under stirring;
(4) under stirring, with ultraviolet lamp irradiation, 2～50 hours time;
(5) under stirring, drip ethyl orthosilicate;
(6) under stirring, will be through adding with the auxiliary nano titanium dioxide powder that soaks into of ethanol and ultrasonic wave, and continuous stirring 1～3 hour;
The organic titanium colloidal sol with photocatalytic activity that (7) will prepare leaves standstill and got final product in 24 hours.
6, the preparation method of a kind of photocatalyst composite according to claim 1 is characterized in that: carrying out low sintering temperature is 150～300 degree.
7, the preparation method of a kind of photocatalyst composite according to claim 1 is characterized in that: the photocatalyst activity composition accounts for 4～10% of gross weight in the photocatalyst composite of making.
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