CN102430386A - Photocatalytic aerogel contained bamboo charcoal-based adsorption and decomposition agent as well as its preparation method - Google Patents
Photocatalytic aerogel contained bamboo charcoal-based adsorption and decomposition agent as well as its preparation method Download PDFInfo
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- CN102430386A CN102430386A CN2011102741071A CN201110274107A CN102430386A CN 102430386 A CN102430386 A CN 102430386A CN 2011102741071 A CN2011102741071 A CN 2011102741071A CN 201110274107 A CN201110274107 A CN 201110274107A CN 102430386 A CN102430386 A CN 102430386A
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Abstract
The invention discloses a preparation method of a photocatalytic aerogel contained bamboo charcoal-based adsorption and decomposition agent. The method comprises the steps of: 1) dissolving tetrabutyl orthotitanate in ethanol, then adding bamboo charcoal particles, and conducting ultrasonic treatment and standing, thus obtaining a mixed solution A; 2) dissolving a chelating agent into an alcohol-water solution so as to obtain a mixed solution B; 3) adding the mixed solution B into the mixed solution A, then adding a drying control chemical additive and conducting stirring, thus obtaining a mixture C; 4) subjecting the mixture C to water bath, aging, absolute ethyl alcohol washing, immersion in a surface modifier solution and immersion in a low surface tension solvent in order; 5) carrying out heat preservation to the substance obtained in step 4) at a temperature of 65-80DEG C for 8-14h first, then performing heat treatment in a nitrogen atmosphere furnace at a temperature of 350-500DEG C for 4-6h, and conducting furnace cooling, thus obtaining the bamboo charcoal-based adsorption and decomposition agent. With good adsorption and decomposition effects, the bamboo charcoal-based adsorption and decomposition agent is hopeful to be used for indoor pollution control, sewage treatment, and other aspects.
Description
Technical field
The present invention relates to a kind of bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge and preparation method thereof, specifically, is a kind of material and production method thereof of decomposing indoor VOCs that be used to adsorb.
Background technology
Bamboo charcoal is fired through the high temperature anaerobic and is formed, and has the abundant microporous structure.From by since being it is found that, just because of absorption, damping, radiation far infrared that it had, discharge function such as anion, and extensively be used in aspects such as house damping, indoor purifying, sewage disposal.And to the adsorptivity that how to improve bamboo charcoal, be the focus that people study always.
TiO
2Aeroge is by nano particle or the mutual coalescence of high-polymer molecular and the cellular solid that constitutes, and the size of its inner hole and basic composition particle all is in nanometer scale, and specific area is at 50~1600m
2/ g, porosity is up to 80%~99.8%, and pore size distribution is even, and light transmission is also better.With TiO
2Powder is different with film, TiO
2Aeroge is transparent or semitransparent shape solid, and ultraviolet light is sweep gas gel particle fully almost, excited gas gel top layer and inner TiO
2, discharge hole and electronics.Constitute TiO in addition
2The basic granules of aeroge is very little; Be in the quantum size scope; When UV-irradiation excited, hole that its surface generates and electronics were difficult for compound, thereby have improved photocatalytic activity greatly; And it is the mesoporous material with high-specific surface area, and pollutant outer surface within it adsorbs simultaneously and degrades.
At present, with bamboo charcoal and TiO
2Compound preparation adsorption decomposition agent has relevant report.The inventor also once was 200710067447.0 " TiO having Ag and multihole at application number
2Modification bamboo charcoal and preparation method thereof " in be to have reported relevant TiO in 201010190411.3 " a kind of adsorption decomposition agent and preparation method thereof " with application number
2Modification bamboo charcoal, and obtained the bamboo charcoal material of better performances.
And with bamboo charcoal and the more excellent TiO of performance
2Aeroge is compound, and relevant report had not also been arranged.In application number was 200810209750.4 " a kind of preparation methods of new control room air pollution ", author Liu Yalan loaded to titania aerogel on the activated carbon fiber, and the material PARA FORMALDEHYDE PRILLS(91,95) degradation rate of preparing reaches 99%.But the emphasis of this patent is how to prepare TiO
2Aeroge.Its shortcoming is to prepare TiO
2Adopt the supercritical drying that cost is higher, technology is complicated in the aeroge process, and unexposed very important how with TiO
2The concrete technology that aeroge and activated carbon fiber are compound.Do not characterize out the specific area of this composite yet.
Summary of the invention
The technical problem that the present invention will solve provide a kind of have that good absorption decomposes effect contain bamboo charcoal base adsorption decomposition agent of photocatalysis aeroge and preparation method thereof.
In order to solve the problems of the technologies described above, the present invention provides a kind of preparation method who contains the bamboo charcoal base adsorption decomposition agent of photocatalysis aeroge, comprises the steps:
1), in 25~50 ℃, butyl titanate is dissolved in the ethanol as solvent, the mol ratio of butyl titanate and ethanol is 1: 1.5~2.5; Add bamboo charcoal particle then, ultrasonic, leave standstill, obtain mixed liquor A;
2), chelating agent is dissolved in mol ratio is that the volume ratio of chelating agent and pure water is 1: 0.8~1.2 in 1: 0.8~1.2 the alcohol solution, stirs, and obtains mixed liquid B;
3), the speed of mixed liquid B with 5~10ml/min is joined in the mixed liquor A control of adding drying then chemical addition agent, stirring 10~60min; Obtain mixture C;
Butyl titanate: chelating agent: the mol ratio of dry control chemical addition agent is 1: 0.5~3.5: 0.5~3.5; The bamboo charcoal consumption accounts for 28~32% of butyl titanate, chelating agent and dry control chemical addition agent gross weight;
4), mixture C is placed 40~70 ℃ of water-bath 6~14h, ageing 1~7d under 40~50 ℃ of temperature again; Then with absolute ethanol washing 1~3 time, use the coating material solution soaking again 1~3 time, soak time is 10~14h at every turn; Soak 1~3 time with low surface tension solvent at last, each soak time is 10~14h;
5), the gains with step 4) are incubated 8~14h down at 65~80 ℃ earlier; Then under 350~500 ℃ of temperature in the nitrogen atmosphere stove heat treatment 4~6h, with stove cooling, load have TiO
2The bamboo charcoal particle of aeroge; This load has TiO
2The bamboo charcoal particle of aeroge is the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge.
Improvement as the preparation method of the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge of the present invention: chelating agent is acetylacetone,2,4-pentanedione, oxalic acid, citric acid, acetic acid, acrylic acid or ethylenediamine.
Further improvement as the preparation method of the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge of the present invention: dry control chemical addition agent is formamide, polyethylene glycol or dimethyl formamide.
Further improvement as the preparation method of the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge of the present invention: the finishing agent solution is that molar concentration is the ethanolic solution of the ethyl orthosilicate of 0.5~2mol/L, the ethanolic solution of trim,ethylchlorosilane or the ethanolic solution of methyl trichlorosilane.
Further improvement as the preparation method of the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge of the present invention: low surface tension solvent is absolute ethyl alcohol, isopropyl alcohol, n-hexane or acetone.
Further improvement as the preparation method of the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge of the present invention: in the step 1): supersonic frequency is 60KHz, and ultrasonic time is 8~12min, and time of repose is 5~10h.
Further improvement as the preparation method of the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge of the present invention: the bamboo charcoal particle particle diameter is 30~50 orders.
In the present invention, step 2) alcohol in the alcohol solution is ethanol.
In the present invention, the butyl titanate branch solves TiO
2
The present invention also provides the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge that utilizes method for preparing and get simultaneously.
The present invention is to bamboo charcoal particle and TiO
2Aeroge carries out reasonably composite, at bamboo charcoal particle surface and the inner normal pressure system photocatalysis titanium dioxide aeroge that adopts, thereby prepare a kind of load TiO is arranged
2The bamboo charcoal material of aerogel particle.
The present invention is that the inventor is at the bamboo charcoal that studies for a long period of time, TiO
2On the basis of aerogel material, obtain through exploring technical process repeatedly.Its advantage is, adopts the original position load technology, makes bamboo charcoal and TiO
2Aeroge composite closely, evenly disperse.Material has combined the absorption and the TiO of bamboo charcoal
2Specific area that aeroge is high and strong photocatalysis effect have reached composite reinforced effects.TiO
2Aeroge is carried in vascular bundle, vessel cluster and the micropore of bamboo charcoal with independent netted form, adopts original position to generate aerogel carried technology, makes load even, and not seeing has reunion.After heat treatment, TiO
2Maintain good anatase crystal.
The present invention is conceived to TiO
2Aerogel carried in bamboo charcoal, and the duct of bamboo charcoal is not stopped up by aeroge; Adopt lower, the simple constant pressure and dry of technology of cost, make full use of TiO
2The advantage of aeroge high-specific surface area, highlight catalytic active, and compound with the renewable resource bamboo charcoal, and one side has improved the adsorption capacity of bamboo charcoal itself greatly, has also reduced independent use TiO on the other hand
2Aeroge is as the cost of adsorbent.
The material that the present invention produced reaches 1200~1600m through its specific area of test
2/ g, being superior at publication number is to report among the CN201010190411.3 " a kind of adsorption decomposition agent and preparation method thereof ".
Press GB 50325-2001 " civil building engineering indoor environmental pollution thing control standard ", GB/T 18204.26-2000 " method for determining formaldehyde in the public place air ", GB/T18204.25-2000 " ammonia assay method in the public place air ", GB11737-89 " benzene, toluene and xylenes health test method-gas chromatography in the atmosphere of residential area " check, record its clearance 99~100%, to the clearance 98~99% of ammonia, to the clearance 97~100% of benzene to free formaldehyde.
Utilize the prepared bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge of the present invention, have good absorption and decompose effect, be expected to be used for aspects such as indoor pollution control, sewage disposal.
The specific embodiment
The particle diameter of the bamboo charcoal particle of being selected for use in following examples is 30~50 orders.
Embodiment 1, a kind of its preparation method that contains the bamboo charcoal base adsorption decomposition agent of photocatalysis aeroge;
Press material molar ratio, butyl titanate: chelating agent: dry control chemical addition agent is 1: 3.5: 3.5.Chelating agent is an acetylacetone,2,4-pentanedione, and dry control chemical addition agent is a formamide, and coating material is the ethanolic solution (concentration is 1mol/L) of ethyl orthosilicate, and low surface tension solvent is an absolute ethyl alcohol.The consumption of bamboo charcoal particle is 30% of butyl titanate, chelating agent and a dry control chemical addition agent weight sum.
Carry out following steps successively:
1), under 25 ℃ of temperature, butyl titanate is dissolved in the ethanol as solvent; Adding bamboo charcoal particle then, is ultrasonic 10min among the 60KHz in frequency, leaves standstill 10h, obtains mixed liquor A; The mol ratio of butyl titanate and ethanol is 1: 2.
2), with ethanol and water mixed in molar ratio according to 1: 1, alcohol solution.
Chelating agent is dissolved in the above-mentioned alcohol solution, stirs, obtain mixed liquid B.The volume ratio of chelating agent and alcohol solution is 1: 1.
3), the speed of mixed liquid B with 5ml/min is joined in the mixed liquor A control of adding drying then chemical addition agent stirring 10min; Obtain mixture C;
4), mixture C is placed 40 ℃ of water-bath 6h, ageing 1d under 40 ℃ of temperature again; Then with absolute ethanol washing 3 times, use the coating material solution soaking again 2 times, soak time is 12h at every turn; Soak 2 times with low surface tension solvent at last, each soak time is 12h; Above-mentioned immersion must guarantee that all mixture C is by submergence.
5), the gains with step 4) are incubated 8h down at 65 ℃ earlier; Then under 350 ℃ of temperature in the nitrogen atmosphere stove heat treatment 4h, with stove cooling, load have TiO
2The bamboo charcoal particle of aeroge; This is loaded with TiO
2The bamboo charcoal particle of aeroge is the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge.
This load has TiO
2The bamboo charcoal particle of aeroge is through test, and its specific area reaches 1350m
2/ g is to the clearance 99% of free formaldehyde, to the clearance 99% of ammonia, to the clearance 97% of benzene.
Embodiment 2, a kind of its preparation method that contains the bamboo charcoal base adsorption decomposition agent of photocatalysis aeroge;
Press material molar ratio, butyl titanate: chelating agent: dry control chemical addition agent is 1: 2.5: 2.5.Chelating agent is an acetic acid, and dry control chemical addition agent is a dimethyl formamide, and coating material is the ethanolic solution (concentration is 1.5mol/L) of methyl trichlorosilane, and the low surface tension solvent of replacement is an isopropyl alcohol at last.The consumption of bamboo charcoal particle is butyl titanate, chelating agent, dry 30% of the chemical addition agent weight sum of controlling.
Carry out following steps successively:
1), under 30 ℃ of temperature, butyl titanate is dissolved in the ethanol as solvent; Adding bamboo charcoal particle then, is ultrasonic 10min among the 60KHz in frequency, leaves standstill 7h, obtains mixed liquor A; The mol ratio of butyl titanate and ethanol is 1: 2,
2), ethanol is mixed according to 1: 1 volume ratio with water, alcohol solution.
Chelating agent is dissolved in the above-mentioned alcohol solution, stirs, obtain mixed liquid B.The volume ratio of chelating agent and pure water is 1: 1.
3), the speed of mixed liquid B with 10ml/min is joined in the mixed liquor A control of adding drying then chemical addition agent stirring 60min; Obtain mixture C;
4), mixture C is placed 40 ℃ of water-bath 14h, ageing 3d under 50 ℃ of temperature again; Then with absolute ethanol washing 3 times, use the coating material solution soaking again 2 times, soak time is 12h at every turn; Soak 3 times with low surface tension solvent at last, each soak time is 12h; Above-mentioned immersion must guarantee that all mixture C is by submergence.
5), the gains with step 4) are incubated 14h down at 80 ℃ earlier; Then under 450 ℃ of temperature in the nitrogen atmosphere stove heat treatment 4h, with stove cooling, load have TiO
2The bamboo charcoal particle of aeroge; This is loaded with TiO
2The bamboo charcoal particle of aeroge is the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge.
This load has TiO
2The bamboo charcoal particle of aeroge is through test, and its specific area reaches 1600m
2/ g is to the clearance 100% of free formaldehyde, to the clearance 99% of ammonia, to the clearance 100% of benzene.
Embodiment 3, a kind of its preparation method that contains the bamboo charcoal base adsorption decomposition agent of photocatalysis aeroge;
Press material molar ratio, butyl titanate: chelating agent: dry control chemical addition agent is 1: 0.5: 0.5.Chelating agent is a citric acid, and dry control chemical addition agent is a dimethyl formamide, and coating material is the ethanolic solution (concentration is 1.8mol/L) of trim,ethylchlorosilane, and the low surface tension solvent of replacement is a n-hexane at last.The consumption of bamboo charcoal particle is 30% of butyl titanate, chelating agent and a dry control chemical addition agent weight sum
Carry out following steps successively:
1), under 50 ℃ of temperature, butyl titanate is dissolved in the ethanol as solvent; Adding bamboo charcoal particle then, is ultrasonic 10min among the 60KHz in frequency, leaves standstill 5h, obtains mixed liquor A; The mol ratio of butyl titanate and ethanol is 1: 2,
2), ethanol is mixed according to 1: 1 volume ratio with water, alcohol solution.
Chelating agent is dissolved in the above-mentioned alcohol solution, stirs, obtain mixed liquid B.The volume ratio of chelating agent and pure water is 1: 1.
3), the speed of mixed liquid B with 10ml/min is joined in the mixed liquor A control of adding drying then chemical addition agent stirring 10min; Obtain mixture C;
4), mixture C is placed 60 ℃ of water-bath 9h, ageing 4d under 40 ℃ of temperature again; Then with absolute ethanol washing 1 time, use the coating material solution soaking again 2 times, soak time is 12h at every turn; Soak 3 times with low surface tension solvent at last, each soak time is 12h; Above-mentioned immersion must guarantee that all mixture C is by submergence.
5), the gains with step 4) are incubated 10h down at 70 ℃ earlier; Then under 500 ℃ of temperature in the nitrogen atmosphere stove heat treatment 4h, with stove cooling, load have TiO
2The bamboo charcoal particle of aeroge; This is loaded with TiO
2The bamboo charcoal particle of aeroge is the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge.
This load has TiO
2The bamboo charcoal particle of aeroge is through test, and its specific area reaches 1570m
2/ g is to the clearance 100% of free formaldehyde, to the clearance 98% of ammonia, to the clearance 99% of benzene.
Embodiment 4, a kind of its preparation method that contains the bamboo charcoal base adsorption decomposition agent of photocatalysis aeroge;
Press material molar ratio, butyl titanate: chelating agent: dry control chemical addition agent is 1: 3: 3.5.Chelating agent is an ethylenediamine, and dry control chemical addition agent is a dimethyl formamide, and coating material is the ethanolic solution (concentration is 0.6mol/L) of methyl trichlorosilane, and the low surface tension solvent of replacement is an acetone at last.The consumption of bamboo charcoal particle is 30% of butyl titanate, chelating agent and a dry control chemical addition agent weight sum
Carry out following steps successively:
1), under 50 ℃ of temperature, butyl titanate is dissolved in the ethanol as solvent; Adding bamboo charcoal particle then, is ultrasonic 10min among the 60KHz in frequency, leaves standstill 10h, obtains mixed liquor A; The mol ratio of butyl titanate and ethanol is 1: 2.
2), ethanol is mixed according to 1: 1 volume ratio with water, alcohol solution.
Chelating agent is dissolved in the above-mentioned alcohol solution, stirs, obtain mixed liquid B.The volume ratio of chelating agent and pure water is 1: 1.
3), the speed of mixed liquid B with 10ml/min is joined in the mixed liquor A control of adding drying then chemical addition agent stirring 60min; Obtain mixture C;
4), mixture C is placed 70 ℃ of water-bath 14h, ageing 7d under 50 ℃ of temperature again; Then with absolute ethanol washing 3 times, use the coating material solution soaking again 3 times, soak time is 12h at every turn; Soak 3 times with low surface tension solvent at last, each soak time is 12h; Above-mentioned immersion must guarantee that all mixture C is by submergence.
5), the gains with step 4) are incubated 14h down at 80 ℃ earlier; Then under 500 ℃ of temperature in the nitrogen atmosphere stove heat treatment 6h, with stove cooling, load have TiO
2The bamboo charcoal particle of aeroge; This is loaded with TiO
2The bamboo charcoal particle of aeroge is the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge.
This load has TiO
2The bamboo charcoal particle of aeroge is through test, and its specific area reaches 1490m
2/ g is to the clearance 99% of free formaldehyde, to the clearance 99% of ammonia, to the clearance 98% of benzene.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (8)
1. contain the preparation method of the bamboo charcoal base adsorption decomposition agent of photocatalysis aeroge, it is characterized in that comprising the steps:
1), in 25~50 ℃, butyl titanate is dissolved in the ethanol as solvent, the mol ratio of butyl titanate and ethanol is 1: 1.5~2.5; Add bamboo charcoal particle then, ultrasonic, leave standstill, obtain mixed liquor A;
2), chelating agent is dissolved in mol ratio is that the volume ratio of said chelating agent and pure water is 1: 0.8~1.2 in 1: 0.8~1.2 the alcohol solution, stirs, and obtains mixed liquid B;
3), the speed of mixed liquid B with 5~10ml/min is joined in the mixed liquor A control of adding drying then chemical addition agent, stirring 10~60min; Obtain mixture C;
Said butyl titanate: chelating agent: the mol ratio of dry control chemical addition agent is 1: 0.5~3.5: 0.5~3.5; The bamboo charcoal consumption accounts for 28~32% of butyl titanate, chelating agent and dry control chemical addition agent gross weight;
4), mixture C is placed 40~70 ℃ of water-bath 6~14h, ageing 1~7d under 40~50 ℃ of temperature again; Then with absolute ethanol washing 1~3 time, use the coating material solution soaking again 1~3 time, soak time is 10~14h at every turn; Soak 1~3 time with low surface tension solvent at last, each soak time is 10~14h;
5), the gains with step 4) are incubated 8~14h down at 65~80 ℃ earlier; Then under 350~500 ℃ of temperature in the nitrogen atmosphere stove heat treatment 4~6h, with stove cooling, load have TiO
2The bamboo charcoal particle of aeroge; This load has TiO
2The bamboo charcoal particle of aeroge is the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge.
2. the preparation method who contains the bamboo charcoal base adsorption decomposition agent of photocatalysis aeroge according to claim 1, it is characterized in that: said chelating agent is acetylacetone,2,4-pentanedione, oxalic acid, citric acid, acetic acid, acrylic acid or ethylenediamine.
3. the preparation method who contains the bamboo charcoal base adsorption decomposition agent of photocatalysis aeroge according to claim 2 is characterized in that: said dry control chemical addition agent is formamide, polyethylene glycol or dimethyl formamide.
4. the preparation method who contains the bamboo charcoal base adsorption decomposition agent of photocatalysis aeroge according to claim 3 is characterized in that: said finishing agent solution is that molar concentration is the ethanolic solution of the ethyl orthosilicate of 0.5~2mol/L, the ethanolic solution of trim,ethylchlorosilane or the ethanolic solution of methyl trichlorosilane.
5. the preparation method who contains the bamboo charcoal base adsorption decomposition agent of photocatalysis aeroge according to claim 4, it is characterized in that: said low surface tension solvent is absolute ethyl alcohol, isopropyl alcohol, n-hexane or acetone.
6. the preparation method who contains the bamboo charcoal base adsorption decomposition agent of photocatalysis aeroge according to claim 5, it is characterized in that: in the said step 1): supersonic frequency is 60KHz, and ultrasonic time is 8~12min, and time of repose is 5~10h.
7. the preparation method who contains the bamboo charcoal base adsorption decomposition agent of photocatalysis aeroge according to claim 6, it is characterized in that: said bamboo charcoal particle particle diameter is 30~50 orders.
8. utilize the bamboo charcoal base adsorption decomposition agent that contains the photocatalysis aeroge that gets like any one method preparation in the claim 1~7.
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CN108467121A (en) * | 2018-05-14 | 2018-08-31 | 胡敏 | A kind of microorganism sewage water processing method being inoculated with flora using activated sludge |
CN109859953A (en) * | 2017-11-30 | 2019-06-07 | 北京化工大学 | A kind of preparation method of bamboo matrix activated carbon/manganese aerogel composite |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103086426A (en) * | 2013-01-14 | 2013-05-08 | 浙江大学 | Preparation method of titanium dioxide aerogel |
CN106268659A (en) * | 2016-04-21 | 2017-01-04 | 浙江海洋学院 | A kind of industrial waste water purifying agent and preparation method thereof |
CN109859953A (en) * | 2017-11-30 | 2019-06-07 | 北京化工大学 | A kind of preparation method of bamboo matrix activated carbon/manganese aerogel composite |
DE102018003805A1 (en) * | 2018-05-11 | 2019-11-14 | Abcr Gmbh | Activated carbon composition and its use for the removal of microplastic particles from water and / or a body of water and / or for the purification of water and / or a body of water |
CN108467121A (en) * | 2018-05-14 | 2018-08-31 | 胡敏 | A kind of microorganism sewage water processing method being inoculated with flora using activated sludge |
CN108467121B (en) * | 2018-05-14 | 2020-11-10 | 金涛 | Microbial sewage treatment method adopting activated sludge to inoculate flora |
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