CN106390351B - A kind of efficient degradation method of polybrominated diphenyl ethers based flame retardant - Google Patents
A kind of efficient degradation method of polybrominated diphenyl ethers based flame retardant Download PDFInfo
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Abstract
The invention discloses a kind of efficient degradation methods of polybrominated diphenyl ethers based flame retardant, the specific steps of the biodegrading process are as follows: surfactant is added in the fire retardant of Xiang Suoshu, it is then added in microwave reactor, 1~2h is heated in 250~300 DEG C of non-pulse microwave continuous, polybrominated biphenyls ethers is promoted to activate and be enriched with, then microwave reflecting device is placed in ultrasound environments and sponge iron/Ag bimetallic catalyst is added, and it is passed through hydrogen, then the strong illumination microwave reactor for being 50000lux with intensity is degraded polybrominated diphenyl ethers based flame retardant by reduction reaction.Biodegrading process of the invention utilizes sponge iron/Ag bimetallic catalyst mating surface activating agent by the efficient degrading polybrominated diphenyl etherss class of reduction reaction energy, and method is simple, and degradation efficiency is high.
Description
Technical field
The present invention relates to environmental protection technical fields, and in particular to a kind of efficient degradation side of polybrominated diphenyl ethers based flame retardant
Method.
Background technique
Polybrominated diphenyl ethers (abbreviation PBDEs) has 209 kinds of homologues such as tetrabromo Biphenyl Ether, pentabromo-, hexabromo, eight bromines, ten bromines.
Polybrominated diphenyl ethers is a kind of brominated flame-retardant haveing excellent performance, and is widely used in various industry and consumer products, while more
Bromo biphenyl ether is also a kind of persistent organic pollutant, highly stable in the environment, difficult to degrade, and has highly lipophilic, low
Water solubility has bioaccumulation and can be enriched with along food chain.At present about the degradation of polybrominated diphenyl ethers and technology for eliminating
Research has been subjected to widely paying attention to.
Polybrominated diphenyl ethers is our traditional fire retardant kinds, and the polybrominated diphenyl ethers kind of industrialized production has: tetrabromo connection
Phenylate, pentabromo- Biphenyl Ether, hexabromobiphenyl ether, seven bromo biphenyl ethers, octa-BDE, nine bromo biphenyl ethers and decabromodiphenyl oxide, wherein
It is commonly three pentabromo- Biphenyl Ether, octa-BDE and decabromodiphenyl oxide kinds.An a kind of major class as bromide fire retardant
Fire retardant matter has been more and more widely used in various consumer products due to its excellent flame retardant property.
Studies have shown that PBDEs significantly risen in various environmental matrices even in multiple proportion increase, animal even
Human fatty tissue, blood, breast milk have detection, therefore have become a kind of pollutant ubiquitous in the ecosystem.It is right
The influence of human body is the study found that the worker's thyroid function for being engaged in production PBDEs obviously weakens.PBDEs under certain condition, can
Being changed into toxic more bromo Er Ben that can be carcinogenic, (PBDFs) and more bromos two and two are disliked Bing Misaki mutters.
Summary of the invention
It is fast, high-efficient and not will cause the more of environmental pollution that the technical problem to be solved in the present invention is to provide a kind of speed
The efficient degradation method of bromo biphenyl ethers fire retardant.
In order to solve the above technical problems, the technical solution adopted by the present invention are as follows:
A kind of specific steps of the efficient degradation method of polybrominated diphenyl ethers based flame retardant are as follows: be added in the fire retardant of Xiang Suoshu
Relative to the surfactant of fire retardant weight percent 0.1%, it is then added in microwave reactor, it is non-at 250~300 DEG C
Pulse microwave 1~2h of laser heating promotes polybrominated biphenyls ethers to activate and be enriched with, microwave reflecting device is then placed in ultrasound environments
In and sponge iron/Ag bimetallic catalyst relative to 0.2 times of quality of fire retardant is added, and press 0.05~0.08m3The speed of/h
It is passed through hydrogen, while the strong illumination microwave reactor for being 50000lux with intensity, by reduction reaction by polybrominated biphenyls ethers
Fire retardant degradation.
Further, the surfactant is lauryl sodium sulfate, sldium lauryl sulfate, sodium glycocholate, poly- second
For glycol to two kinds of mixture any in isooctyl phenyl ether, mixed proportion is mass ratio 1:1.
Further, surface is provided on the chemical reaction equipment in the microwave reactor contain 35% in-situ preparation
Cu TiO2 conduction band, wherein irradiation of the Cu by strong light, Cu ion, which can capture on TiO2 conduction band light excitation and generate, to be reduced
Electronics, polybrominated diphenyl ethers based flame retardant can by TiO2 conduction band by light activated Hole oxidation, the more bromines connection of simultaneous catalytic reduction
Phenylate.
Further, magnetic stirrer is also contained in the microwave reactor, mixing speed is continuously adjustable and shows in real time
Show.
Further, the ultrasonic frequency in the ultrasound environments is 25KHz~40KHz.
Further, the sponge iron/Ag bimetallic catalyst the preparation method comprises the following steps: by sponge iron be immersed in relative to
In the deionized water of 10 times of sponge iron amounts, the silver nitrate solution measured relative to 5 times of sponge iron is then added and is stirred under ultrasound environments
It mixes to fully reacting, filtering removes excessive silver nitrate solution, is subsequently placed in magnetic separator and carries out Magnetic Isolation, spend after separation
Ionized water is cleaned multiple times, and is then dried under vacuum up to the sponge iron/Ag bimetallic catalyst.
Further, the polybrominated biphenyls ethers degraded in microwave reactor is cooled in mass ratio 8 after 25~40 DEG C:
1 adds the bacterial strain of pseudomonad and anaerobic fungi bacterial strain thereto, and 24~36h is stood in closed environment, carries out biological drop
Solution.Biodegrade can prevent chemical degradation incomplete, can a greater degree of degrading polybrominated diphenyl etherss based flame retardant.
The beneficial effects of the present invention are embodied in: the present invention utilizes sponge iron/Ag bimetallic catalyst mating surface activating agent
Auxiliary is with microwave reactor, and surfactant can guarantee that polybrominated biphenyls ethers is activated and is enriched with, sponge iron/Ag bimetallic catalyst
With preferable dispersibility and surface energy, in addition by electrostatic force, the effect of surface tension under ultrasound environments, to polybrominated diphenyl ethers
Class has good reducing power, and microwave reactor can promote reaction speed, and can be heated by non-pulse microwave continuous, protects
Polybrominated biphenyls ethers efficient-decomposition is demonstrate,proved.
Specific embodiment
Embodiment 1
A kind of efficient degradation method of polybrominated diphenyl ethers based flame retardant, the specific steps of the biodegrading process are as follows: to institute
The surfactant relative to fire retardant 0.1% is added in the fire retardant stated, is then added in microwave reactor, at 250 DEG C
Non-pulse microwave continuous heats 1h, promotes polybrominated biphenyls ethers to activate and be enriched with, microwave reflecting device is then placed in ultrasound environments
In and sponge iron/Ag bimetallic catalyst relative to 0.2 times of quality of fire retardant is added, and press 0.05m3The speed of/h is passed through hydrogen
Gas, the strong illumination microwave reactor for being then 50000lux with intensity, by reduction reaction by polybrominated diphenyl ethers based flame retardant
Decompose removal.
Wherein, the surfactant is lauryl sodium sulfate, two kinds of sldium lauryl sulfate of mixture；Mixing ratio
Example is mass ratio 1:1.Surface is provided on chemical reaction equipment in the microwave reactor, and to contain 35% generated in-situ
The TiO2 conduction band of Cu, wherein irradiation of the Cu by strong light, Cu ion can capture light excitation generation on TiO2 conduction band and be reduced
Electronics, polybrominated diphenyl ethers based flame retardant can by TiO2 conduction band by light activated Hole oxidation, simultaneous catalytic reduction polybrominated biphenyls
Ethers；Also contain magnetic stirrer, the continuously adjustable simultaneously real-time display of mixing speed in the microwave reactor；The ultrasound
Ultrasonic frequency in environment is 25KHz.
Wherein, the sponge iron/Ag bimetallic catalyst is the preparation method comprises the following steps: be immersed in deionized water for sponge iron
In, excessive silver nitrate solution is then added and is stirred under ultrasound environments to fully reacting, it is molten that filtering removes excessive silver nitrate
Liquid, is subsequently placed in magnetic separator and carries out Magnetic Isolation, be cleaned multiple times after separation with deionized water, is then dried under vacuum to obtain the final product
The sponge iron/Ag bimetallic catalyst.
Wherein, the polybrominated biphenyls ethers degraded in microwave reactor is cooled to after 25 DEG C 8:1 in mass ratio thereto
The bacterial strain and anaerobic fungi bacterial strain for adding pseudomonad stand for 24 hours in closed environment, carry out biodegrade.Biodegrade
Chemical degradation can be prevented incomplete, it can a greater degree of degrading polybrominated diphenyl etherss based flame retardant.
Embodiment 2
A kind of efficient degradation method of polybrominated diphenyl ethers based flame retardant, the specific steps of the biodegrading process are as follows: to institute
The surfactant relative to fire retardant 0.1% is added in the fire retardant stated, is then added in microwave reactor, at 275 DEG C
Non-pulse microwave continuous heats 1.5h, promotes polybrominated biphenyls ethers to activate and be enriched with, microwave reflecting device is then placed in ultrasonic ring
In border and sponge iron/Ag bimetallic catalyst relative to 0.2 times of quality of fire retardant is added, and presses 0.065m3The speed of/h is logical
Enter hydrogen, the strong illumination microwave reactor for being then 50000lux with intensity is hindered polybrominated biphenyls ethers by reduction reaction
It fires agent and decomposes removal.
Wherein, the surfactant is sodium glycocholate, polyethylene glycol to two kinds of isooctyl phenyl ether of mixture；It is mixed
Composition and division in a proportion example is mass ratio 1:1.It is provided with surface on chemical reaction equipment in the microwave reactor and contains 35% life in situ
At Cu TiO2 conduction band, wherein irradiation of the Cu by strong light, Cu ion, which can capture on TiO2 conduction band light excitation and generate, to be gone back
Former electronics, polybrominated diphenyl ethers based flame retardant can by TiO2 conduction band by light activated Hole oxidation, the more bromines of simultaneous catalytic reduction
Biphenyl Ether；Also contain magnetic stirrer, the continuously adjustable simultaneously real-time display of mixing speed in the microwave reactor；Described is super
Ultrasonic frequency in acoustic environment is 32.5KHz.
Wherein, the sponge iron/Ag bimetallic catalyst is the preparation method comprises the following steps: be immersed in deionized water for sponge iron
In, excessive silver nitrate solution is then added and is stirred under ultrasound environments to fully reacting, it is molten that filtering removes excessive silver nitrate
Liquid, is subsequently placed in magnetic separator and carries out Magnetic Isolation, be cleaned multiple times after separation with deionized water, is then dried under vacuum to obtain the final product
The sponge iron/Ag bimetallic catalyst.
Wherein, by the polybrominated biphenyls ethers degraded in microwave reactor be cooled to after 32.5 DEG C 8:1 in mass ratio to its
In add the bacterial strain and anaerobic fungi bacterial strain of pseudomonad, 30h is stood in closed environment, carries out biodegrade.Biology drop
Solution can prevent chemical degradation incomplete, can a greater degree of degrading polybrominated diphenyl etherss based flame retardant.
Embodiment 3
A kind of efficient degradation method of polybrominated diphenyl ethers based flame retardant, the specific steps of the biodegrading process are as follows: to institute
The surfactant relative to fire retardant 0.1% is added in the fire retardant stated, is then added in microwave reactor, at 300 DEG C
Non-pulse microwave continuous heats 2h, promotes polybrominated biphenyls ethers to activate and be enriched with, microwave reflecting device is then placed in ultrasound environments
In and sponge iron/Ag bimetallic catalyst relative to 0.2 times of quality of fire retardant is added, and press 0.08m3The speed of/h is passed through hydrogen
Gas, the strong illumination microwave reactor for being then 50000lux with intensity, by reduction reaction by polybrominated diphenyl ethers based flame retardant
Decompose removal.
Wherein, the surfactant is lauryl sodium sulfate, polyethylene glycol mixes two kinds of isooctyl phenyl ether
Close object；Mixed proportion is mass ratio 1:1.Surface, which is provided with, on chemical reaction equipment in the microwave reactor contains 35%
The TiO2 conduction band of generated in-situ Cu, wherein irradiation of the Cu by strong light, Cu ion can capture light excitation on TiO2 conduction band and produce
The raw electronics being reduced, polybrominated diphenyl ethers based flame retardant, by light activated Hole oxidation, while can be catalyzed also on TiO2 conduction band
Former polybrominated diphenyl ethers；Also contain magnetic stirrer, the continuously adjustable simultaneously real-time display of mixing speed in the microwave reactor；Institute
The ultrasonic frequency in ultrasound environments stated is 40KHz.
Wherein, the sponge iron/Ag bimetallic catalyst is the preparation method comprises the following steps: be immersed in deionized water for sponge iron
In, excessive silver nitrate solution is then added and is stirred under ultrasound environments to fully reacting, it is molten that filtering removes excessive silver nitrate
Liquid, is subsequently placed in magnetic separator and carries out Magnetic Isolation, be cleaned multiple times after separation with deionized water, is then dried under vacuum to obtain the final product
The sponge iron/Ag bimetallic catalyst
Wherein, the polybrominated biphenyls ethers degraded in microwave reactor is cooled to after 40 DEG C 8:1 in mass ratio thereto
The bacterial strain and anaerobic fungi bacterial strain for adding pseudomonad stand 36h in closed environment, carry out biodegrade.Biodegrade
Chemical degradation can be prevented incomplete, it can a greater degree of degrading polybrominated diphenyl etherss based flame retardant.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify to technical solution documented by previous embodiment or equivalent replacement of some of the technical features；And
These are modified or replaceed, the spirit and model of technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution
It encloses.
Claims (3)
1. a kind of efficient degradation method of polybrominated diphenyl ethers based flame retardant, which is characterized in that the specific step of the biodegrading process
Suddenly are as follows: the surfactant relative to fire retardant weight percent 0.1% is added in the fire retardant of Xiang Suoshu, is then added to micro-
In wave reactor, 1~2h is heated in 250~300 DEG C of non-pulse microwave continuous, promotes polybrominated biphenyls ethers to activate and be enriched with, so
Microwave reactor is placed in ultrasound environments afterwards and sponge iron/Ag bimetallic catalytic relative to 0.2 times of quality of fire retardant is added
Agent, and it is passed through hydrogen, while the strong illumination microwave reactor for being 50000lux with intensity by the speed of 0.05~0.08m3/h,
Polybrominated diphenyl ethers based flame retardant is degraded by reduction reaction；
The surfactant is lauryl sodium sulfate, sldium lauryl sulfate, sodium glycocholate, polyethylene glycol to iso-octyl benzene
Any two kinds of mixture in base ether, mixed proportion are mass ratio 1:1；
The TiO2 that 35% generated in-situ Cu is contained on surface is provided on chemical reaction equipment in the microwave reactor to lead
Band；
Also contain magnetic stirrer, the continuously adjustable simultaneously real-time display of mixing speed in the microwave reactor；
The sponge iron/Ag bimetallic catalyst is measured the preparation method comprises the following steps: being immersed in sponge iron relative to 10 times of sponge iron
Deionized water in, be then added relative to 5 times of sponge iron measure silver nitrate solution stirred under ultrasound environments to fully reacting,
Filtering, which is placed in magnetic separator, carries out Magnetic Isolation, is cleaned multiple times, is then dried under vacuum with deionized water after separation to obtain the final product
The sponge iron/Ag bimetallic catalyst.
2. a kind of efficient degradation method of polybrominated diphenyl ethers based flame retardant as described in claim 1, it is characterised in that: described
Ultrasonic frequency in ultrasound environments is 25KHz~40KHz.
3. a kind of efficient degradation method of polybrominated diphenyl ethers based flame retardant as described in claim 1, which is characterized in that will be micro-
The polybrominated biphenyls ethers degraded in wave reactor is cooled to 8:1 in mass ratio after 25~40 DEG C and adds pseudomonad thereto
The hybrid bacterial strain of bacterial strain and anaerobic fungi bacterial strain stands 24~36h in closed environment, carries out biodegrade.
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| CN113462679A (en) * | 2021-06-30 | 2021-10-01 | 生态环境部华南环境科学研究所 | Method for degrading polybrominated diphenyl ether flame retardant by utilizing biological sponge iron |
| CN113913853B (en) * | 2021-11-23 | 2023-06-23 | 浙江工业大学 | Electrochemical deep degradation method for brominated phenolic compounds under synergistic adsorption of surfactant |
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| CN102351297A (en) * | 2011-09-15 | 2012-02-15 | 山东大学 | Treatment method of halogenated organic pollutant waste water |
| CN102502985A (en) * | 2011-10-25 | 2012-06-20 | 南京大学 | Method for removing typical bromide flame retardant based on Fe/Ag reduction-class Fenton oxidization |
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| CN102351297A (en) * | 2011-09-15 | 2012-02-15 | 山东大学 | Treatment method of halogenated organic pollutant waste water |
| CN102533582A (en) * | 2011-09-20 | 2012-07-04 | 北京师范大学 | Efficient degradation bacteria for PBDEs (polybrominated diphenyl ethers) and application thereof |
| CN102502985A (en) * | 2011-10-25 | 2012-06-20 | 南京大学 | Method for removing typical bromide flame retardant based on Fe/Ag reduction-class Fenton oxidization |
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| 还原-氧化两步处理法降解水中典型溴代阻燃剂的研究;罗斯;《中国博士学位论文全文数据库（电子期刊） 工程科技I辑》;20111015;同上 |
| 还原-氧化两步处理法降解水中典型溴代阻燃剂的研究;罗斯;《中国博士学位论文全文数据库（电子期刊） 工程科技I辑》;20111015;第7页第3段，第17页最后1段-第18页第1段，第23页第2.1.2节，第44页第1段，48页最后1段-49页第1段，55页第1段，56页第1段，第67页第1段 |
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