CN109607726A - A method of degradation phosphonium flame retardant waste water - Google Patents
A method of degradation phosphonium flame retardant waste water Download PDFInfo
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- CN109607726A CN109607726A CN201811445948.2A CN201811445948A CN109607726A CN 109607726 A CN109607726 A CN 109607726A CN 201811445948 A CN201811445948 A CN 201811445948A CN 109607726 A CN109607726 A CN 109607726A
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- waste water
- flame retardant
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- phosphonium flame
- cyclodextrin
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The present invention relates to a kind of methods of phosphonium flame retardant waste water of degrading, include the following steps: that compound drug is taken to add by 0.1 ‰~0.5 ‰ waste water weight percents into phosphonium flame retardant waste water, adjust pH to 2~7, it is put into constant temperature oscillator, adjust the temperature to 20~40 DEG C, revolving speed is 100~200rpm, vibrates 0.5~2.5h；It is taken out from constant temperature oscillator, adds liquid dephosphorization agent by 1 ‰~2 ‰ waste water weight percents, be uniformly mixed, after standing reaction a period of time, adjusted pH to neutrality, stand a period of time, take remaining total phosphorus concentration in sample supernatant detection waste water.The multi step strategy method that the present invention uses, first by organic phosphorus and polymeric form the Phos in adsorbent material waste water, then by flocculation sedimentation Phos, it is finally reached the purpose of efficiently removal total phosphorus, and selection absorption-flocculation sedimentation-such waste water of flocculation sedimentation three-step approach processing, effect are more preferable.
Description
Technical field
The invention belongs to technical field of waste water processing, concretely relate to a kind of side of phosphonium flame retardant waste water of degrading
Method.
Background technique
Since phosphorus flame retardant uses the features such as extensive, pollution is big, strong toxicity, phosphonium flame retardant waste water is not only to ring
Border causes seriously to pollute, while seriously endangering people's health, and problems more have aroused widespread concern in all circles of society,
Therefore there is huge social environment benefit to the processing of such waste water, selects a kind of suitable method instantly to handle water environment
In fire retardant pollutant be very urgent and necessary.
At present in Treatment of Industrial Water, absorption method have adsorption rate is fast, operation is simple, adsorbed product recoverable,
It the advantages that secondary pollution will not being generated to environment, early in the last century 70's just by common concern, obtains more and more extensive
Application.
A kind of adsorbent of the absorbent charcoal material as function admirable, since its chemical property is stablized, high mechanical strength is resistance to
It is sour, alkaline-resisting, heat-resisting, not soluble in water and organic solvent, the features such as use can be regenerated, so that absorbent charcoal material is in water treatment field
It is paid high attention to, and has carried out a large amount of research work.Zhang Cunfang et al. research shows that active carbon to Cu in waste water2+、Ni2+
Eliminating rate of absorption respectively reach 86.60% and 76.08% (bibliography: Shandong chemical industry, 2018,47 (04): 144-146).
The researchs such as Wu Yue adsorb phenol wastewater using Activated Carbon with Cu (Cu/GAC), as a result, it has been found that Activated Carbon with Cu (Cu/GAC) is to 4-NP
95.2% and 89.5% (bibliography: water purification technology, 2018 (09): 101-105) is respectively reached with the removal rate of phenol.China
Patent CN 102247804A discloses a kind of preparation method for loading and having the activated carbon fibre dephosphorization agent of lanthanum hydroxide.
It is applied in waste water treatment for active carbon and activated carbon modified material, the country has many patents, but due to work
The property many reasons such as charcoal price and method of modifying complexity, and the absorption of phosphonium flame retardant waste water is not studied systematically.It examines
Consider the plurality of advantages of absorbent charcoal material, therefore for the removal containing phosphor contaminant in phosphorus flame retardant waste water, passes through active carbon
Material, which carries out research to the absorption of phosphonium flame retardant, has certain realistic meaning.
Summary of the invention
In order to overcome the deficiencies in the prior art, it is useless that the purpose of the present invention is to provide a kind of degradation phosphonium flame retardants
The method of water.
The technical solution adopted by the present invention are as follows:
A method of degradation phosphonium flame retardant waste water includes the following steps:
(1) in prepared composition comprising beta-cyclodextrin, bentonite, active carbon compound drug, it is spare；
(2) in prepared composition comprising sodium, iron, lanthanum element liquid dephosphorization agent, it is spare；
(3) it takes compound drug to add by 0.1 ‰~0.5 ‰ waste water weight percents into phosphonium flame retardant waste water, adjusts
PH to 2~7, is put into constant temperature oscillator, adjusts the temperature to 20~40 DEG C, and revolving speed is 100~200rpm, vibrates 0.5~2.5h；
(4) it is taken out from constant temperature oscillator, adds liquid dephosphorization agent by 1 ‰~2 ‰ waste water weight percents, mixing is equal
It is even, after standing reaction a period of time, adjusts pH to neutrality, stand a period of time, take remaining total in sample supernatant detection waste water
Phosphorus concentration.
Preferably, the compound drug is prepared as follows:
(a) beta-cyclodextrin is added into water, is dissolved under conditions of 40~80 DEG C with magnetic stirrer；
(b) bentonite is added into above-mentioned solution, with magnetic stirrer, filter residue is dried to obtain β-ring paste by filtering
Essence-Bent；
(c) above-mentioned beta-cyclodextrin-Bent is added in active carbon, be uniformly mixed up to compound drug.
Preferably, the mass ratio of beta-cyclodextrin and water is 1:300~600 in step (a).
Preferably, the mass ratio of bentonite and water is 1:8~15 in step (b)；Mixing time is after bentonite is added
1.5~5.5h, the control of filter residue drying temperature are 50~70 DEG C.
Preferably, the mass ratio of active carbon and beta-cyclodextrin-Bent are 1:2.5~5.5 in step (c).
Preferably, the liquid dephosphorization agent is prepared as follows: it is molten that sodium sulfite being added to iron chloride
It in liquid, is uniformly mixed, adds lanthanum chloride solution, be stirred to react, after ultrasound, then stand, filter and liquid dephosphorization agent is made.
Preferably, the mass ratio of the sodium sulfite, iron chloride, lanthanum chloride is 1:5~30:0.00002~0.0002.
Preferably, described be stirred to react the time as 1~3h, time of repose is 10~15h.
Preferably, the compound drug is prepared as follows:
(a) 0.1g beta-cyclodextrin is added into 50mL water, is dissolved under conditions of 60 DEG C with magnetic stirrer；
(b) 5g bentonite is added into above-mentioned solution, with magnetic stirrer 3h, filtering, by filter residue in 60 DEG C of items
It is dried under part, obtains beta-cyclodextrin-Bent；
(c) above-mentioned beta-cyclodextrin-Bent is added by 25% activated carbon weight percentage, is uniformly mixed up to compound medicine
Agent；
The liquid dephosphorization agent is prepared as follows:
The sodium sulfite of 2.5g is added in the ferric chloride solution of 50mL40%, is uniformly mixed, adding 2mL concentration is
The lanthanum chloride solution of 0.05g/L is stirred to react 2 hours, ultrasound a period of time, then stands 12 hours, filters and liquid dephosphorization is made
Agent.
Preferably, the method for the degradation phosphonium flame retardant waste water: being added by 0.3 ‰ waste water weight percents above-mentioned
The compound drug of preparation adjusts pH to 3, is put into constant temperature oscillator, adjusts the temperature to 30 DEG C, revolving speed 160rpm, vibrates 2h；It takes
Out, the liquid dephosphorization agent of above-mentioned preparation is added by 1 ‰ waste water weight percents, is uniformly mixed, and after standing reaction 30min, is adjusted
PH stands a period of time, takes remaining total phosphorus concentration in sample supernatant detection waste water to neutrality.
Compared with prior art, the invention has the following advantages:
(1) the multi step strategy method that the present invention uses passes through the organic phosphorus and polymeric form in adsorbent material waste water first
Phos be finally reached the purpose of efficiently removal total phosphorus then by flocculation sedimentation Phos, and select absorption-flocculation heavy
Shallow lake-such the waste water of flocculation sedimentation three-step approach processing, effect are more preferable；
(2) the compound drug preparation method that the present invention uses is simple, and raw material is easy to get cheaply, and compound drug is for organic phosphorus
And the Phos effect of polymeric form is more preferable, so that the dosage of active carbon reduces, cost is effectively reduced；
(3) the liquid dephosphorization agent preparation method that the present invention uses is simple, and preparation cost is low, without pressurization and heating, application
Prospect is good, meets environmental-friendly and circular economy requirement.
Specific embodiment
The present invention is further explained in the light of specific embodiments, but invention which is intended to be protected is not limited to
This.
Embodiment 1
Compound drug is prepared as follows:
(a) 0.1g beta-cyclodextrin is added into 50mL water, is dissolved under conditions of 60 DEG C with magnetic stirrer；
(b) 5g bentonite is added into above-mentioned solution, with magnetic stirrer 3h, filtering, by filter residue in 60 DEG C of items
It is dried under part, obtains beta-cyclodextrin-Bent；
(c) above-mentioned beta-cyclodextrin-Bent is added by 25% activated carbon weight percentage, is uniformly mixed up to compound medicine
Agent.
Liquid dephosphorization agent is prepared as follows:
The sodium sulfite of 2.5g is added in the ferric chloride solution of 50mL40%, is uniformly mixed, adding 2mL concentration is
The lanthanum chloride solution of 0.05g/L is stirred to react 2 hours, ultrasound a period of time, then stands 12 hours, filters and liquid dephosphorization is made
Agent.
Company, Zhejiang Province phosphonium flame retardant waste water is taken, answering for above-mentioned preparation is added by 0.3 ‰ waste water weight percents
Dose out powders adjust pH to 3, are put into constant temperature oscillator, adjust the temperature to 30 DEG C, revolving speed 160rpm, vibrate 0.5h；It takes out, by 2 ‰
Waste water weight percent adds the liquid dephosphorization agent of above-mentioned preparation, is uniformly mixed, and after standing reaction 1h, adjusts pH to neutrality, quiet
A period of time is set, remaining total phosphorus concentration in sample supernatant detection waste water is taken.The result shows that the removal rate of Phosphorus From Wastewater is
84.67%.
Embodiment 2
It is similar with the process of embodiment 1, but pH to 7 is adjusted after compound drug is added, remaining step is identical, the results showed that, it gives up
The removal rate of phosphorus is 80.05% in water.
Embodiment 3
It is similar with the process of embodiment 1, but duration of oscillation is 2h, remaining step is identical, the results showed that, Phosphorus From Wastewater is gone
Except rate is 87.88%.
Embodiment 4
It is similar with the process of embodiment 3, but pH to 7 is adjusted after compound drug is added, remaining step is identical, the results showed that, it gives up
The removal rate of phosphorus is 84.55% in water.
Embodiment 5
Compound drug is prepared as follows:
(a) 0.1g beta-cyclodextrin is added into 50mL water, is dissolved under conditions of 60 DEG C with magnetic stirrer；
(b) 5g bentonite is added into above-mentioned solution, with magnetic stirrer 3h, filtering, by filter residue in 60 DEG C of items
It is dried under part, obtains beta-cyclodextrin-Bent；
(c) above-mentioned beta-cyclodextrin-Bent is added by 25% activated carbon weight percentage, is uniformly mixed up to compound medicine
Agent.
Liquid dephosphorization agent is prepared as follows:
The sodium sulfite of 2.5g is added in the ferric chloride solution of 50mL40%, is uniformly mixed, adding 2mL concentration is
The lanthanum chloride solution of 0.05g/L is stirred to react 2 hours, ultrasound a period of time, then stands 12 hours, filters and liquid dephosphorization is made
Agent.
Company, Zhejiang Province phosphonium flame retardant waste water is taken, answering for above-mentioned preparation is added by 0.3 ‰ waste water weight percents
Dose out powders adjust pH to 3, are put into constant temperature oscillator, adjust the temperature to 30 DEG C, revolving speed 160rpm, vibrate 0.5h；It takes out, by 1 ‰
Waste water weight percent adds the liquid dephosphorization agent of above-mentioned preparation, is uniformly mixed, and after standing reaction 30min, then presses 1 ‰ waste water
Weight percent adds the liquid dephosphorization agent of above-mentioned preparation, and after standing reaction 30min, tune pH to neutrality stands a period of time,
Take remaining total phosphorus concentration in sample supernatant detection waste water.The result shows that the removal rate of Phosphorus From Wastewater is 90.76%.
Embodiment 6
It is similar with 5 process of embodiment, but pH to 7 is adjusted after compound drug is added, remaining step is identical, the results showed that, waste water
The removal rate of middle phosphorus is 85.05%.
Embodiment 7
It is similar with the process of embodiment 5, but duration of oscillation is 2h, remaining step is identical, the results showed that, Phosphorus From Wastewater is gone
Except rate is 94.23%.
Embodiment 8
It is similar with the process of embodiment 7, but pH to 7 is adjusted after compound drug is added, remaining step is identical, the results showed that, it gives up
The removal rate of phosphorus is 90.53% in water.
Claims (10)
1. a kind of method for phosphonium flame retardant waste water of degrading, it is characterised in that include the following steps:
(1) in prepared composition comprising beta-cyclodextrin, bentonite, active carbon compound drug, it is spare；
(2) in prepared composition comprising sodium, iron, lanthanum element liquid dephosphorization agent, it is spare；
(3) it takes compound drug to add by 0.1 ‰~0.5 ‰ waste water weight percents into phosphonium flame retardant waste water, adjusts pH to 2
~7, it is put into constant temperature oscillator, adjusts the temperature to 20~40 DEG C, revolving speed is 100~200rpm, vibrates 0.5~2.5h；
(4) it is taken out from constant temperature oscillator, adds liquid dephosphorization agent by 1 ‰~2 ‰ waste water weight percents, be uniformly mixed, it is quiet
After setting reaction a period of time, adjusts pH to neutrality, stand a period of time, take remaining total phosphorus in sample supernatant detection waste water dense
Degree.
2. the method for phosphonium flame retardant waste water of degrading according to claim 1, it is characterised in that the compound drug is according to such as
Lower method is prepared:
(a) beta-cyclodextrin is added into water, is dissolved under conditions of 40~80 DEG C with magnetic stirrer；
(b) bentonite is added into above-mentioned solution, with magnetic stirrer, filter residue is dried to obtain beta-cyclodextrin-by filtering
Bent；
(c) above-mentioned beta-cyclodextrin-Bent is added in active carbon, be uniformly mixed up to compound drug.
3. the method for phosphonium flame retardant waste water of degrading according to claim 2, it is characterised in that: in step (a), beta-cyclodextrin
Mass ratio with water is 1:300~600.
4. according to claim 3 degrade phosphonium flame retardant waste water method, it is characterised in that: in step (b), bentonite with
The mass ratio of water is 1:8~15；Mixing time is 1.5~5.5h after bentonite is added, and the control of filter residue drying temperature is 50~70
℃。
5. according to claim 4 degrade phosphonium flame retardant waste water method, it is characterised in that: in step (c), active carbon with
The mass ratio of beta-cyclodextrin-Bent is 1:2.5~5.5.
6. according to claim 1 degrade phosphonium flame retardant waste water method, it is characterised in that the liquid dephosphorization agent according to
Following method is prepared: sodium sulfite being added in ferric chloride solution, is uniformly mixed, adds lanthanum chloride solution, is stirred
Reaction after ultrasonic, then is stood, and filters and liquid dephosphorization agent is made.
7. the method for phosphonium flame retardant waste water of degrading according to claim 6, it is characterised in that: the sodium sulfite, chlorination
Iron, lanthanum chloride mass ratio be 1:5~30:0.00002~0.0002.
8. the method for phosphonium flame retardant waste water of degrading according to claim 7, it is characterised in that: described to be stirred to react the time and be
1~3h, time of repose are 10~15h.
9. the method for phosphonium flame retardant waste water of degrading according to claim 1, it is characterised in that the compound drug is according to such as
Lower method is prepared:
(a) 0.1g beta-cyclodextrin is added into 50mL water, is dissolved under conditions of 60 DEG C with magnetic stirrer；
(b) 5g bentonite is added into above-mentioned solution, with magnetic stirrer 3h, filtering, by filter residue under the conditions of 60 DEG C
Drying, obtains beta-cyclodextrin-Bent；
(c) above-mentioned beta-cyclodextrin-Bent is added by 25% activated carbon weight percentage, is uniformly mixed up to compound drug；
The liquid dephosphorization agent is prepared as follows:
The sodium sulfite of 2.5g is added in the ferric chloride solution of 50mL40%, is uniformly mixed, adding 2mL concentration is
The lanthanum chloride solution of 0.05g/L is stirred to react 2 hours, ultrasound a period of time, then stands 12 hours, filters and liquid dephosphorization is made
Agent.
10. the method for phosphonium flame retardant waste water of degrading according to claim 9, it is characterised in that: press 0.3 ‰ waste water weight hundred
The compound drug of above-mentioned preparation is added in point ratio, adjusts pH to 3, is put into constant temperature oscillator, adjusts the temperature to 30 DEG C, revolving speed is
160rpm vibrates 2h；It takes out, the liquid dephosphorization agent of above-mentioned preparation is added by 1 ‰ waste water weight percents, be uniformly mixed, it is quiet
After setting reaction 30min, adjusts pH to neutrality, stand a period of time, take remaining total phosphorus concentration in sample supernatant detection waste water.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104291420A (en) * | 2014-09-11 | 2015-01-21 | 陕西省石油化工研究设计院 | Phosphorus removing agent containing inorganic mineral and application method thereof |
| CN106430549A (en) * | 2016-08-31 | 2017-02-22 | 维克·恩格拜 | Sewage ordered treatment method |
| CN106698548A (en) * | 2017-01-14 | 2017-05-24 | 冯志祥 | High-efficient phosphate removing agent and preparation method thereof |
| CN108773941A (en) * | 2018-07-10 | 2018-11-09 | 无锡锐众环保科技有限公司 | A kind of processing method of Electronics Factory's high phosphorus high-nitrogen waste water |
-
2018
- 2018-11-29 CN CN201811445948.2A patent/CN109607726A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012176618A1 (en) * | 2011-06-20 | 2012-12-27 | 富士フイルム株式会社 | Water purification method |
| CN104291420A (en) * | 2014-09-11 | 2015-01-21 | 陕西省石油化工研究设计院 | Phosphorus removing agent containing inorganic mineral and application method thereof |
| CN106430549A (en) * | 2016-08-31 | 2017-02-22 | 维克·恩格拜 | Sewage ordered treatment method |
| CN106698548A (en) * | 2017-01-14 | 2017-05-24 | 冯志祥 | High-efficient phosphate removing agent and preparation method thereof |
| CN108773941A (en) * | 2018-07-10 | 2018-11-09 | 无锡锐众环保科技有限公司 | A kind of processing method of Electronics Factory's high phosphorus high-nitrogen waste water |
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Application publication date: 20190412 |