CN102120665A - Method for purifying pentachlorophenol in water through photocatalysis - Google Patents
Method for purifying pentachlorophenol in water through photocatalysis Download PDFInfo
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- CN102120665A CN102120665A CN 201110020264 CN201110020264A CN102120665A CN 102120665 A CN102120665 A CN 102120665A CN 201110020264 CN201110020264 CN 201110020264 CN 201110020264 A CN201110020264 A CN 201110020264A CN 102120665 A CN102120665 A CN 102120665A
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Abstract
The invention relates to a method for purifying pentachlorophenol (PCP) in water through photocatalysis, which comprises the following processes of: mixing and stirring a bismuth silicate photocatalyst and pentachlorophenol sewage to be treated, performing ultrasonic dispersion, adsorbing and balancing, irradiating by using a xenon lamp and the like; and pentachlorophenol photocatalytic degradation reaction results prove that the pentachlorophenol in the water can be efficiently purified through the method. The invention can overcome the defects of high energy consumption, complex operation, violent reaction conditions, poor purification capacity and the like in the conventional purification method, provides a method having the advantages of short flow, simple equipment and good efficiency of purifying the pentachlorophenol, and has wide industrial application prospect.
Description
Technical field
The present invention relates to a kind of purify waste water method of middle Pentachlorophenol (PCP) of bismuth silicate photocatalyst of utilizing, belong to the surround lighting catalysis technical field.
Background technology
Pentachlorophenol (PCP) once was widely used as wood preservative, rust-preventive agent, sterilizing agent, sterilant, sterilant and weedicide, have stench and high toxicity, be a kind ofly extensively to be present in water body and to have " three cause " (carcinogenic, teratogenesis, mutagenesis) effect and genotoxic organic difficult degradation pollutent, be difficult for being decomposed and easily by the food chain enrichment in vivo, thereby natural, ecological and human health are caused serious threat, listed in the list of priority pollutants by EPA.Simultaneously, PCP can also be converted into stronger many chloros dibenzo Dioxins (PCDDs) of toxicity and polychlorinated dibenzo (PCDFs) in physical environment, and it is crucial therefore seeking economy and eco-friendly PCP purification techniques.
Shortcomings such as biological process is a kind of effective ways of PCP in purifying waste water, and have the low and easy-operating advantage of cost, but this method exists long processing period, and big and high density PCP processing efficiency is low to the effect of microorganism toxicity.Physico-chemical process mainly comprises absorption method, Coagulation Method, extraction process and membrane processing method etc.This method only is PCP from a kind of medium to the process that another kind of medium shifts, and can produce new pollution usually, therefore needs subsequent processes just can reach the purpose of thorough removing PCP.The Sonochemical degradation method exists capacity usage ratio low, and treatment capacity is little, problems such as process cost height.Wet oxidation process needs high-tension apparatus, the apparatus cost costliness, and catalyst attrition is big, and uneconomical to lower concentration PCP wastewater treatment.There are shortcomings such as current efficiency is low, power consumption is high and lack electrode life in the electrochemical degradation method owing to be subjected to the restriction of electrode materials, therefore is difficult to realize industrialization.
The photocatalytic degradation technology is the novel method of Persistent organic pollutants in a kind of purifying water body that grows up the seventies, have that energy consumption is low, easy to operate, reaction conditions is gentle, oxidation capacity is strong, with advantage such as environmental compatible, utilizing this technology to purify organic wastewater with difficult degradation thereby has become the domestic and international research focus.Photocatalyst can produce electron-hole pair under illumination condition, valence band hole (h
+ Vb) have very strong oxidation capacity, can efficiently remove organism in the water; Be adsorbed on the O of catalyst surface simultaneously
2And H
2O can produce various living radicals with the conduction band electron reaction, as hydroxyl radical free radical (OH), ultra-oxygen anion free radical (O
2 -) etc., redox reaction can take place with PCP in these living radicals, is translated into the low material of toxicity or is carbonic acid gas and water with its mineralising, thereby effectively degrade PCP, has wide prospect in industrial application.
Bi silicate crystals is the non-ferroelectric cube semiconductor of a kind of broad-band gap, high resistivity, has unique photoelectricity, photoconduction, light and sells off and the acousto-optic performance.In recent years, as a kind of important photoelectric material, bi silicate crystals has caused the great attention of Materials science and photocatalysis field.The patent No. is ZL 200710166218.4, and name is called a kind of preparation method of bismuth silicate powder photocatalyst, and publication number is the preparation method that the patent of CN101157026A describes bismuth silicate in detail.Document " C.H.He, M.Y.Gu.Preparation, characterization and photocatalytic properties of Bi
12SiO
20Powders ScriptaMaterialia 2006 (55): 481-484 " adopt chemical solution decomposition method (CSD) preparation bismuth silicate powder; and investigate its performance Congo red to photocatalytic degradation, the result show illumination after one hour bismuth silicate to Congo red decolorizing efficiency up to 92.1%.
Problem to be solved by this invention is efficiently to remove PCP pollutent in the water, overcomes the existing deficiency that purifies the chlorophenol pollutant technology, and a kind of treatment process of chlorophenols sewage efficient, energy-conservation, simple to operate is provided.
Summary of the invention
The objective of the invention is to solve the pollution problem of PCP in the Industrial processes, providing a kind of is the method for PCP during photocatalyst is purified waste water with the bismuth silicate, can overcome existing purifying method energy consumption height, complicated operation, reaction conditions is violent and the shortcoming of detergent power difference, has good economy and environmental benefit.
Utilize bismuth silicate for photocatalyst purify waste water in the method for PCP comprise the steps:
A) the certain density PCP solution of preparation;
B) in PCP solution, add the bismuth silicate photocatalyst;
C) under the dark condition ultrasonic 10 minutes, make the bismuth silicate photocatalyst be dispersed in PCP solution;
D) with c) mixing solutions of step stirs to reach the adsorption equilibrium of PCP at the dark condition lower magnetic force;
E) adopt xenon lamp to shine, the temperature of reaction solution keeps constant temperature by water-bath simultaneously;
F) timing sampling, sample thief supernatant liquor after the centrifugation, the change in concentration of analysis PCP;
G) suction filtration reaction solution, the Separation and Recovery photocatalyst.
The treatment process of PCP sewage of the present invention wherein, is 2～10 mg/litre at the starting point concentration of PCP described in the step a);
The treatment process of PCP sewage of the present invention wherein, is 300～800 nanometers in the xenon lamp wavelength region described in the step e), and power is 500 watts;
Among the present invention, the photocatalysis apparatus that is adopted is made up of direct supply, barretter and xenon lamp, and miscellaneous part comprises quartz reactor, water-bath and magnetic stirring apparatus etc., and used unit all can obtain from relevant device supplier, also can design voluntarily and build.
Analytical procedure to PCP in the water provided by the invention is as follows:
Adopt high performance liquid chromatography (HPLC Waters 1525) to analyze, moving phase is the mixed solution of the methyl alcohol and the amine acetate aqueous solution (containing 0.02 mol amine acetate), volume ratio is 85: 15, flow velocity 1.0 ml/min, it is 312 nanometers that UV-detector is measured wavelength, and specimen is removed impurity in order to avoid stop up pillar through 0.45 micron filter membrane.Degradation rate (%)=(initial p CP concentration-residue PCP concentration)/initial p CP concentration * 100%.
The invention has the advantages that:
1. adopt luminous energy to remove PCP in the water, efficiently utilize clean energy;
2. can efficiently remove the pollution of difficult degradation PCP in the water;
3. this method flow is short, equipment is simple, easy to operate, purification rate is high, photocatalyst is recycled easily, has good economic benefit and environmental benefit.
This method is that the 250 mg/litre PCP sewage that to handle 200 milliliters of starting point concentrations be 2 mg/litre is after 2 hours at the photocatalyst consumption, almost can't detect on high performance liquid chromatography PCP, and photocatalyst can reused more than 5 times under the prerequisite that does not reduce catalytic effect.
Description of drawings
Fig. 1 for utilize bismuth silicate for photocatalyst purify waste water in the different starting point concentration PCP processes concentration (wherein catalyst consumption is 250 mg/litre, pH=6.12) over time.
Embodiment
Embodiment 1
In 50 milligrams of bismuth silicate powders PCP solution that to be scattered in 200 milliliters of starting point concentrations be 2 mg/litre, under dark condition,, catalyzer is disperseed fully in solution with ultrasonic 10 minutes of mixed solution.Pre-irradiation stirs 30 minutes to reach adsorption equilibrium with mixed solution at the dark condition lower magnetic force earlier, uses 500 watts of xenon lamps (wavelength is 300～800 nanometers) to shine then, and conditioned reaction liquid level and xenon lamp lamp holder spacing are 20 centimetres.Magnetic agitation in the process of photocatalytic degradation is so that reaction solution is even, and the temperature of reaction solution remains on (20 ± 2) degree by water-bath.Regularly get 1 ml sample, supernatant liquor is got in centrifugation, and the sampling back uses HPLC to analyze the concentration of PCP.The result shows that after reaction was carried out 2 hours, the degradation rate of PCP was greater than 99.0%.
In 50 milligrams of bismuth silicate powders PCP solution that to be scattered in 200 milliliters of starting point concentrations be 4 mg/litre, under dark condition,, catalyzer is disperseed fully in solution with ultrasonic 10 minutes of mixed solution.Pre-irradiation stirs 30 minutes to reach adsorption equilibrium with mixed solution at the dark condition lower magnetic force earlier, uses 500 watts of xenon lamps (wavelength is 300～800 nanometers) to shine then, and conditioned reaction liquid level and xenon lamp lamp holder spacing are 20 centimetres.Magnetic agitation in the process of photocatalytic degradation is so that reaction solution is even, and the temperature of reaction solution remains on (20 ± 2) degree by water-bath.Regularly get 1 ml sample, get supernatant liquor after the centrifugation, the sampling back uses HPLC to analyze the concentration of PCP.The result shows that after reaction was carried out 2 hours, the degradation rate of PCP reached 87.7%.
Embodiment 3
In 50 milligrams of bismuth silicate powders PCP solution that to be scattered in 200 milliliters of starting point concentrations be 6 mg/litre, under dark condition,, catalyzer is disperseed fully in solution with ultrasonic 10 minutes of mixed solution.Pre-irradiation stirs 30 minutes to reach adsorption equilibrium with mixed solution at the dark condition lower magnetic force earlier, uses 500 watts of xenon lamps (wavelength is 300～800 nanometers) to shine then, and conditioned reaction liquid level and xenon lamp lamp holder spacing are 20 centimetres.Magnetic agitation in the process of photocatalytic degradation is so that reaction solution is even, and the temperature of reaction solution remains on (20 ± 2) degree by water-bath.Regularly get 1 ml sample, get supernatant liquor after the centrifugation, the sampling back uses HPLC to analyze the concentration of PCP.The result shows that after reaction was carried out 2 hours, the degradation rate of PCP reached 84.5%.
In 100 milligrams of bismuth silicate powders PCP solution that to be scattered in 200 milliliters of starting point concentrations be 6 mg/litre, under dark condition,, catalyzer is disperseed fully in solution with ultrasonic 10 minutes of mixed solution.Pre-irradiation stirs 30 minutes to reach adsorption equilibrium with mixed solution at the dark condition lower magnetic force earlier, uses 500 watts of xenon lamps (wavelength is 300～800 nanometers) to shine then, and conditioned reaction liquid level and xenon lamp lamp holder spacing are 20 centimetres.Magnetic agitation in the process of photocatalytic degradation is so that reaction solution is even, and the temperature of reaction solution remains on (20 ± 2) degree by water-bath.Regularly get 1 ml sample, get supernatant liquor after the centrifugation, the sampling back uses HPLC to analyze the concentration of PCP.The result shows that after reaction was carried out 2 hours, the degradation rate of PCP reached 91.2%.
Embodiment 5
In 100 milligrams of bismuth silicate powders PCP solution that to be scattered in 200 milliliters of starting point concentrations be 10 mg/litre, under dark condition,, catalyzer is disperseed fully in solution with ultrasonic 10 minutes of mixed solution.Pre-irradiation stirs 30 minutes to reach adsorption equilibrium with mixed solution at the dark condition lower magnetic force earlier, uses 500 watts of xenon lamps (wavelength is 300～800 nanometers) to shine then, and conditioned reaction liquid level and xenon lamp lamp holder spacing are 20 centimetres.Magnetic agitation in the process of photocatalytic degradation is so that reaction solution is even, and the temperature of reaction solution remains on (20 ± 2) degree by water-bath.Regularly get 1 ml sample, get supernatant liquor after the centrifugation, the sampling back uses HPLC to analyze the concentration of PCP.The result shows that after reaction was carried out 2 hours, the degradation rate of PCP reached 78.1%.
Claims (3)
1. one kind is utilized bismuth silicate to comprise for the purify waste water step of middle Pentachlorophenol (PCP) of photocatalyst:
1) the certain density PCP solution of preparation;
2) in PCP solution, add the bismuth silicate photocatalyst;
3) under the dark condition ultrasonic 10 minutes, the bismuth silicate photocatalyst is dispersed in the PCP solution;
4) the described mixing solutions of step 3) is stirred to reach the adsorption equilibrium of PCP at the dark condition lower magnetic force;
5) adopt xenon lamp to shine, the temperature of reaction solution keeps constant temperature by water-bath simultaneously;
6) timing sampling, sample thief supernatant liquor after the centrifugation, the change in concentration of analysis PCP;
7) suction filtration reaction solution, the Separation and Recovery photocatalyst.
2. according to the purifying method of PCP in the claim 1, wherein, in step 1), the starting point concentration of described PCP is 2～10 mg/litre.
3. according to the method described in the claim 1, it is characterized in that: the light catalytic purifying process 5 of PCP), described xenon lamp wavelength region is 300～800 nanometers, and power is 500 watts xenon lamp.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103551098A (en) * | 2013-11-01 | 2014-02-05 | 合肥工业大学 | Method for generating hydroxyl free radical through controlling visible light |
| CN103771638A (en) * | 2012-10-26 | 2014-05-07 | 北京师范大学 | Photo-catalysis method adopting ultrasonic atomizing process to enhance water pollution treatment effect |
| CN104888401A (en) * | 2015-05-20 | 2015-09-09 | 中国科学院新疆理化技术研究所 | Method for dechlorination from chlorophenol pollutant by using alkali metal zinc borate compound via photocatalysis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157026A (en) * | 2007-11-08 | 2008-04-09 | 北京师范大学 | A preparation method of bismuth silicate powder photocatalyst |
| CN101638253A (en) * | 2009-09-08 | 2010-02-03 | 北京师范大学 | Method for treating waste water polluted by composite chlorophenol with coordination of visible light-laccase |
| CN101891274A (en) * | 2010-07-27 | 2010-11-24 | 北京师范大学 | Method for coprocessing crystal violet polluted sewage by outdoor natural light-hydrogen peroxide |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157026A (en) * | 2007-11-08 | 2008-04-09 | 北京师范大学 | A preparation method of bismuth silicate powder photocatalyst |
| CN101638253A (en) * | 2009-09-08 | 2010-02-03 | 北京师范大学 | Method for treating waste water polluted by composite chlorophenol with coordination of visible light-laccase |
| CN101891274A (en) * | 2010-07-27 | 2010-11-24 | 北京师范大学 | Method for coprocessing crystal violet polluted sewage by outdoor natural light-hydrogen peroxide |
Non-Patent Citations (1)
| Title |
|---|
| 《污染防治技术》 20090228 何莉等 CuO /TiO2 - H2 O2 自然光催化降解印染废水的影响因素 第8-11页 1-3 第22卷, 第1期 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103771638A (en) * | 2012-10-26 | 2014-05-07 | 北京师范大学 | Photo-catalysis method adopting ultrasonic atomizing process to enhance water pollution treatment effect |
| CN103771638B (en) * | 2012-10-26 | 2016-08-10 | 北京师范大学 | A kind of photocatalysis method with ultrasonic atomizatio enhanced sewage treatment effect |
| CN103551098A (en) * | 2013-11-01 | 2014-02-05 | 合肥工业大学 | Method for generating hydroxyl free radical through controlling visible light |
| CN104888401A (en) * | 2015-05-20 | 2015-09-09 | 中国科学院新疆理化技术研究所 | Method for dechlorination from chlorophenol pollutant by using alkali metal zinc borate compound via photocatalysis |
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