CN104192939B - 4-nonyl-phenoxy-dioxygen vinethene decomposing method - Google Patents

4-nonyl-phenoxy-dioxygen vinethene decomposing method Download PDF

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CN104192939B
CN104192939B CN201410489047.9A CN201410489047A CN104192939B CN 104192939 B CN104192939 B CN 104192939B CN 201410489047 A CN201410489047 A CN 201410489047A CN 104192939 B CN104192939 B CN 104192939B
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oxide powder
nonyl
phenoxy
suspension
dioxygen
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CN201410489047.9A
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CN104192939A (en
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宋大鹏
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倪海霞
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Abstract

The invention discloses a 4-nonyl-phenoxy-dioxygen vinethene decomposing method which comprises the following steps: (1) preparing a Mn/Sr/Ba/Zn-oxidized powdered activated carbon nanometer material; (2) decomposing 4-nonyl-phenoxy-dioxygen vinethene: adding the Mn/Sr/Ba/Zn-oxidized powdered activated carbon nanometer material prepared in the step (1) into 4-nonyl-phenoxy-dioxygen vinethene wastewater with the concentration of 1-50<Mu>g/L, regulating the pH to 6-8, radiating with visible light for 120-150 minutes under the condition of sonic oscillation, introducing oxygen into the wastewater at the same time to aerate, wherein the amount of the added Mn/Sr/Ba/Zn-oxidized powdered activated carbon nanometer material is 4-10g/L; and (3) measuring the degradation rate of the 4-nonyl-phenoxy-dioxygen vinethene. The method is simple in process and convenient in operation, the water containing estrogen is industrially treated, the biotoxicity of the estrogen is eliminated, the method is particularly suitable for eliminating the toxicity of drugs in a water body, and the removal rate of the estrogen in the water is up to 99% when the 4-nonyl-phenoxy-dioxygen vinethene sewage is treated.

Description

A kind of method of decomposing 4-nonyl-phenoxy group-dioxygen Vinyl Ether
Technical field
The present invention relates to a kind of method of decomposing 4-nonyl-phenoxy group-dioxygen Vinyl Ether, belong to field of environment protection.
Background technology
Environmental estrogens (Enviromental Estrogens, EEs) is that a class has estrogen activity, can simulate the physiology of endogenous estrogen, biochemical action, or has the xenobiotics of effect of antagonism male hormone.Environmental estrogens of a great variety, is extensively present in the various environment that the mankind can contact, and enters animals and human beings body by food or biologic chain.At present, the oestrogenic hormon kind had been found that comprises: the medicinal oestrogenic hormon, plant estrogen, fungoid oestrogenic hormon, pesticide oestrogenic hormon, industrial chemical oestrogen-like hormone, metal species oestrogenic hormon etc. of synthetic.Except phytoestrogen is a kind ofly conducive to except the environmental estrogens of HUMAN HEALTH, other most of environmental estrogens all can affect the Development of Reproductive System of animal body and neurotoxic effect may be produced, cause disease of immune system, induced tumor generates morbidity etc..
The degraded product of ionic surface active agent alkylphenol polyoxyethylene (A P E s) has estrogen activity, which results in the great attention of people, because APEs is widely used in work, agriculture production and daily life, environmental pollution widely.In the industrial production, the purposes of A PE s mainly comprises plastics and plastelast production process, textile mills' washing, destarch, bleaching, resination production technique, agricultural chemicals humidification, emulsification production technique, paper mill slurrying production process.Wherein 4-nonyl-phenoxy group-dioxygen Vinyl Ether (NP2EO) is a kind of typical A P E s material.
In current removal water body, the method for oestrogenic hormon bio-toxicity (as middle 4-nonyl-phenoxy group-dioxygen Vinyl Ether) is divided into substantially:
1, adopt A/O method, i.e. anoxic/aerobic method process combined is containing estrogenic water.This method processing cost is low, but is not easily biodegradable due to oestrogenic hormon, builds this equipment and effectively can not remove estrogenic bio-toxicity in water.
2., adopt active carbon adsorption process containing estrogenic water.This method process can be adsorbed onto activated carbon surface magnetic hormone from water, but can not remove the toxicity of such material, and processing cost is high, measures less, needs to regularly replace sorbent material, easily produces secondary pollution.
3, adopt membrane technology process containing estrogenic water.This method retains trace estrogen in water body, but can not remove the toxicity of such material, and film easily blocks, and need periodic replacement, processing cost is high, measures less.
4, estrogenic water is contained with the process of UV ozone advanced oxidation processes.This method detoxification successful, but UV ozone advanced oxidation processes to estrogenic removal and mineralization ability limited, and treatment capacity is little.
And aforesaid method is not good for the pollutant effluents treatment effect of micro-concentrations.
Summary of the invention
For above-mentioned prior art Problems existing, the invention provides a kind of method of decomposing 4-nonyl-phenoxy group-dioxygen Vinyl Ether, comprise the steps:
(1), the preparation of Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material
Take Powdered Activated Carbon as raw material, under 8 DEG C of conditions, Powdered Activated Carbon 6-8g slowly being joined concentration is in the vitriol oil 20-45mL of 98%, rapid stirring 30min, slowly add 8-16g potassium bichromate again and stir 10min, under 20 DEG C of constant temperature after sonic oscillation 1h, add pure water dilution, obtain suspension, the further magnesium oxide/absorbent charcoal of 100-200ml ozone is passed in suspension, dry in 90 DEG C of constant temperature ovens again, by 2KW microwave, filter to obtain oxide powder gac; By oxide powder gac 0.1-0.2g and MnO 2nano powder 0.15-0.18g joins in 150-200mL distilled water, adds dispersion agent ultrasonic disperse 1h, obtains oxide powder gac suspension; By the SrCl of 2.5-3.0g 26H 2o slowly joins in oxide powder gac suspension, stirs 20 minutes, then by the CeCl of 0.4-0.6g 36H 2o slowly adds in oxide powder gac suspension, stirred at ambient temperature 20 minutes, then by the BaCl of 0.6-0.9g 22H 2o slowly adds in oxide powder gac suspension, then by the ZnCl of 0.3-0.5g 2slowly add in oxide powder gac suspension, stirred at ambient temperature 20 minutes, regulator solution, to neutral, obtains mixing suspension; Filter to obtain solid matter, washing 3-5 time, dries 2h at 90 DEG C, and grinding, obtains Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material;
(2), the decomposition of 4-nonyl-phenoxy group-dioxygen Vinyl Ether
It is in the 4-nonyl-phenoxy group-dioxygen Vinyl Ether waste water of 1-50 μ g/L that Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material step (1) prepared adds concentration, adjust pH is 6-8, with radiation of visible light 120-150 minute under the condition of sonic oscillation, in waste water, pass into oxygen carries out aeration simultaneously, and Mn/Sr/ Ce/Ba/Zn-oxide powder gac nano material add-on is 4-10g/L;
(3) degradation rate of 4-nonyl-phenoxy group-dioxygen Vinyl Ether, is measured.
The oxide powder quality of activated carbon added in step (1) is 0.15g, MnO 2nano powder quality is 0.16g, SrCl 26H 2the quality of O is 2.8g, CeCl 36H 2the quality of O is 0.5g, BaCl 22H 2the quality of O is 0.8g, ZnCl 2quality be 0.4g.
In step (2), the radiation of visible light time is 135 minutes.
In step (2), the frequency of sonic oscillation is 40KHz.
The invention has the advantages that:
(1) present invention process is simple, easy to operate, industrial treatment can contain estrogenic water, remove estrogenic bio-toxicity, be specially adapted to the toxicity removing water body Chinese traditional medicine, when sewage for 4-nonyl-phenoxy group-dioxygen Vinyl Ether processes, estrogenic clearance in water can be made to reach 99%.
(2) the raw materials used dosage of the present invention is little, is general inorganic reagent, cheap and easy to get; Reaction is carried out at normal temperatures and pressures, and system is simple; Degradation process is rapid, and after 120 minutes, degradation efficiency is close to maximum;
(3) the present invention is applicable to the removal of polluting environmental estrogens in various natural water body and artificial water by estrogens, and for the sewage water body of micro-concentrations, clearance also can reach 98%.
Embodiment
embodiment 1
(1), the preparation of Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material
Take Powdered Activated Carbon as raw material, under 8 DEG C of conditions, Powdered Activated Carbon 6g slowly being joined concentration is in the vitriol oil 20mL of 98%, rapid stirring 30min, slowly add 8g potassium bichromate again and stir 10min, under 20 DEG C of constant temperature after sonic oscillation 1h, add pure water dilution, obtain suspension, the further magnesium oxide/absorbent charcoal of 100ml ozone is passed in suspension, dry in 90 DEG C of constant temperature ovens again, by 2KW microwave, filter to obtain oxide powder gac; By oxide powder gac 0.1g and MnO 2nano powder 0.15g joins in 150mL distilled water, adds dispersion agent ultrasonic disperse 1h, obtains oxide powder gac suspension; By the SrCl of 2.5g 26H 2o slowly joins in oxide powder gac suspension, stirs 20 minutes, then by the CeCl of 0.4g 36H 2o slowly adds in oxide powder gac suspension, stirred at ambient temperature 20 minutes, then by the BaCl of 0.6g 22H 2o slowly adds in oxide powder gac suspension, then by the ZnCl of 0.3g 2slowly add in oxide powder gac suspension, stirred at ambient temperature 20 minutes, regulator solution, to neutral, obtains mixing suspension; Filter to obtain solid matter, wash 3 times, at 90 DEG C, dry 2h, grinding, obtains Mn/Sr/ Ce/Ba/Zn-oxide powder gac nano material;
(2), the decomposition of 4-nonyl-phenoxy group-dioxygen Vinyl Ether
It is in the 4-nonyl-phenoxy group-dioxygen Vinyl Ether waste water of 50 μ g/L that Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material step (1) prepared adds concentration, adjust pH is 6-8, radiation of visible light 150 minutes are used under the sonic oscillation condition that frequency is 40KHz, in waste water, pass into oxygen carries out aeration simultaneously, and Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material add-on is 10g/L;
(3) degradation rate, measuring 4-nonyl-phenoxy group-dioxygen Vinyl Ether reaches 98%.
embodiment 2
(1), the preparation of Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material
Take Powdered Activated Carbon as raw material, under 8 DEG C of conditions, Powdered Activated Carbon 8g slowly being joined concentration is in the vitriol oil 45mL of 98%, rapid stirring 30min, slowly add 16g potassium bichromate again and stir 10min, under 20 DEG C of constant temperature after sonic oscillation 1h, add pure water dilution, obtain suspension, the further magnesium oxide/absorbent charcoal of 200ml ozone is passed in suspension, dry in 90 DEG C of constant temperature ovens again, by 2KW microwave, filter to obtain oxide powder gac; By oxide powder gac 0.2g and MnO 2nano powder 0.18g joins in 200mL distilled water, adds dispersion agent ultrasonic disperse 1h, obtains oxide powder gac suspension; By the SrCl of 3.0g 26H 2o slowly joins in oxide powder gac suspension, stirs 20 minutes, then by the CeCl of 0.6g 36H 2o slowly adds in oxide powder gac suspension, stirred at ambient temperature 20 minutes, then by the BaCl of 0.9g 22H 2o slowly adds in oxide powder gac suspension, then by the ZnCl of 0.5g 2slowly add in oxide powder gac suspension, stirred at ambient temperature 20 minutes, regulator solution, to neutral, obtains mixing suspension; Filter to obtain solid matter, wash 5 times, at 90 DEG C, dry 2h, grinding, obtains Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material;
(2), the decomposition of 4-nonyl-phenoxy group-dioxygen Vinyl Ether
It is in the 4-nonyl-phenoxy group-dioxygen Vinyl Ether waste water of 1 μ g/L that Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material step (1) prepared adds concentration, adjust pH is 6-8, radiation of visible light 120 minutes are used under the sonic oscillation condition that frequency is 40KHz, in waste water, pass into oxygen carries out aeration simultaneously, and Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material add-on is 4g/L;
(3) degradation rate, measuring 4-nonyl-phenoxy group-dioxygen Vinyl Ether reaches 98%
embodiment 3
(1), the preparation of Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material
Take Powdered Activated Carbon as raw material, under 8 DEG C of conditions, Powdered Activated Carbon 7g slowly being joined concentration is in the vitriol oil 30mL of 98%, rapid stirring 30min, slowly add 12g potassium bichromate again and stir 10min, under 20 DEG C of constant temperature after sonic oscillation 1h, add pure water dilution, obtain suspension, the further magnesium oxide/absorbent charcoal of 150ml ozone is passed in suspension, dry in 90 DEG C of constant temperature ovens again, by 2KW microwave, filter to obtain oxide powder gac; By oxide powder gac 0.15g and MnO 2nano powder 0.16g joins in 180mL distilled water, adds dispersion agent ultrasonic disperse 1h, obtains oxide powder gac suspension; By the SrCl of 2.8g 26H 2o slowly joins in oxide powder gac suspension, stirs 20 minutes, then by the CeCl of 0.5g 36H 2o slowly adds in oxide powder gac suspension, stirred at ambient temperature 20 minutes, then by the BaCl of 0.8g 22H 2o slowly adds in oxide powder gac suspension, then by the ZnCl of 0.4g 2slowly add in oxide powder gac suspension, stirred at ambient temperature 20 minutes, regulator solution, to neutral, obtains mixing suspension; Filter to obtain solid matter, wash 4 times, at 90 DEG C, dry 2h, grinding, obtains Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material;
(2), the decomposition of 4-nonyl-phenoxy group-dioxygen Vinyl Ether
It is in the 4-nonyl-phenoxy group-dioxygen Vinyl Ether waste water of 20 μ g/L that Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material step (1) prepared adds concentration, adjust pH is 6-8, radiation of visible light 135 minutes are used under the sonic oscillation condition that frequency is 40KHz, in waste water, pass into oxygen carries out aeration simultaneously, and Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material add-on is 8g/L;
(3) degradation rate, measuring 4-nonyl-phenoxy group-dioxygen Vinyl Ether reaches 99%.

Claims (4)

1. decompose a method for 4-nonyl-phenoxy group-dioxygen Vinyl Ether, it is characterized in that the method comprises the steps:
(1), the preparation of Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material
Take Powdered Activated Carbon as raw material, under 8 DEG C of conditions, Powdered Activated Carbon being about 6-8g, slowly to join concentration be in the vitriol oil 20-45mL of 98%, rapid stirring 30min, slowly add 8-16g potassium bichromate again and stir 10min, under 20 DEG C of constant temperature after sonic oscillation 1h, add pure water dilution, obtain suspension, the further magnesium oxide/absorbent charcoal of 100-200ml ozone is passed in suspension, dry in 90 DEG C of constant temperature ovens again, by 2KW microwave, filter to obtain oxide powder gac; By oxide powder gac 0.1-0.2g and MnO 2nano powder 0.15-0.18g joins in 150-200mL distilled water, adds dispersion agent ultrasonic disperse 1h, obtains oxide powder gac suspension; By the SrCl of 2.5-3.0g 26H 2o slowly joins in oxide powder gac suspension, stirs 20 minutes, then by the CeCl of 0.4-0.6g 36H 2o slowly adds in oxide powder gac suspension, stirred at ambient temperature 20 minutes, then by the BaCl of 0.6-0.9g 22H 2o slowly adds in oxide powder gac suspension, then by the ZnCl of 0.3-0.5g 2slowly add in oxide powder gac suspension, stirred at ambient temperature 20 minutes, regulator solution, to neutral, obtains mixing suspension; Filter to obtain solid matter, washing 3-5 time, dries 2h at 90 DEG C, and grinding, obtains Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material;
(2), the decomposition of 4-nonyl-phenoxy group-dioxygen Vinyl Ether
It is in the 4-nonyl-phenoxy group-dioxygen Vinyl Ether waste water of 1-50 μ g/L that Mn/Sr/Ce/Ba/Zn-oxide powder gac nano material step (1) prepared adds concentration, adjust pH is 6-8, with radiation of visible light 120-150 minute under the condition of sonic oscillation, in waste water, pass into oxygen carries out aeration simultaneously, and Mn/Sr/ Ce/Ba/Zn-oxide powder gac nano material add-on is 4-10g/L;
(3) degradation rate of 4-nonyl-phenoxy group-dioxygen Vinyl Ether, is measured.
2. the method for decomposition 4-nonyl-phenoxy group-dioxygen Vinyl Ether according to claim 1, it is characterized in that, the oxide powder quality of activated carbon added in step (1) is 0.15g, MnO 2nano powder quality is 0.16g, SrCl 26H 2the quality of O is 2.8g, CeCl 36H 2the quality of O is 0.5g, BaCl 22H 2the quality of O is 0.8g, ZnCl 2quality be 0.4g.
3. the method for decomposition 4-nonyl-phenoxy group-dioxygen Vinyl Ether according to claim 1, it is characterized in that, in step (2), the radiation of visible light time is 135 minutes.
4. the method for decomposition 4-nonyl-phenoxy group-dioxygen Vinyl Ether according to claim 1, it is characterized in that, in step (2), the frequency of sonic oscillation is 40KHz.
CN201410489047.9A 2014-09-23 2014-09-23 4-nonyl-phenoxy-dioxygen vinethene decomposing method CN104192939B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6129849A (en) * 1998-10-23 2000-10-10 Kansai Electric Power Co., Inc. Process for accelerating reaction of ozone with AM catalyst
CN101036886A (en) * 2007-02-09 2007-09-19 南京大学 Application of mesoporous bigger serface titania and zinc oxide
CN101306864A (en) * 2008-06-25 2008-11-19 浙江工业大学 Degradation process for environment estrogenic pollutant in water body
CN101898847A (en) * 2009-05-27 2010-12-01 中国科学院生态环境研究中心 System for treating sewage containing nonylphenol polyoxyethylene ether and metabolin
CN102407128A (en) * 2011-09-21 2012-04-11 青岛农业大学 Preparation method and application of Gd, Pr or Yb doped fenton catalyst

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6129849A (en) * 1998-10-23 2000-10-10 Kansai Electric Power Co., Inc. Process for accelerating reaction of ozone with AM catalyst
CN101036886A (en) * 2007-02-09 2007-09-19 南京大学 Application of mesoporous bigger serface titania and zinc oxide
CN101306864A (en) * 2008-06-25 2008-11-19 浙江工业大学 Degradation process for environment estrogenic pollutant in water body
CN101898847A (en) * 2009-05-27 2010-12-01 中国科学院生态环境研究中心 System for treating sewage containing nonylphenol polyoxyethylene ether and metabolin
CN102407128A (en) * 2011-09-21 2012-04-11 青岛农业大学 Preparation method and application of Gd, Pr or Yb doped fenton catalyst

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