CN104437381A - Attapulgite microwave-organic modification method and method for treating polycyclic aromatic hydrocarbon in oil producing wastewater by utilizing attapulgite - Google Patents
Attapulgite microwave-organic modification method and method for treating polycyclic aromatic hydrocarbon in oil producing wastewater by utilizing attapulgite Download PDFInfo
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- CN104437381A CN104437381A CN201410543704.3A CN201410543704A CN104437381A CN 104437381 A CN104437381 A CN 104437381A CN 201410543704 A CN201410543704 A CN 201410543704A CN 104437381 A CN104437381 A CN 104437381A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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Abstract
The invention discloses an attapulgite microwave-organic modification method and a method for treating polycyclic aromatic hydrocarbon in oil producing wastewater by utilizing attapulgite, and belongs to the technical field of waste reclamation and pollution control. According to the invention, attapulgite acts as a main material, and is subjected to microwave-organic modification, and the obtained adsorbent has relatively high adsorption capacity to polycyclic aromatic hydrocarbon in the oil producing wastewater. The amount of a surfactant, the use amount of attapulgite, the microwave time, the pH of a solution and the reaction temperature all affect the treatment effect. The reserve of attapulgite is very rich in China. Because the traditional adsorbent activated carbon is high in cost, is difficult to regenerate and the like, attapulgite is expected to replace the activated carbon to be an environment-friendly and cheap adsorbent.
Description
Technical field
The present invention relates to the technical field of changing waste into resources utilization and Environmental capacity, be specifically related to the method for a kind of microwave-organically-modified attapulgite and apply the method for polycyclic aromatic hydrocarbon in this attapulgite process oil extraction waste water.
Background technology
In recent years, the water environment of China just suffer from unprecedented severe contamination.In all waste water, oily waste water oneself become very important polluted-water.Oils enters water body environment by different approaches and forms oily waste water, and oily waste water is that a kind of amount is large, wide and endanger serious waste water, and its source is a lot.Industrial oily waste water amount is maximum, and composition is also very complicated, except the impurity that the oil emulsion, solid particle, hydrogen sulfide etc. containing solubility salt and heavy metal, suspension is natural, also containing hydrophobic organic compound polycyclic aromatic hydrocarbon.The compound that IARC (IARC) (1976) 94 kinds of listing are carcinogenic to animal used as test, wherein 15 kinds belong to polycyclic aromatic hydrocarbon.The physical method of conventional removal polycyclic aromatic hydrocarbon has heating, coagulant sedimentation, and chemical method has photooxidation and chemical agent to be oxidized two classes, also has microorganism treatment in addition.But general physics and chemistry method cannot thorough degrading polycyclic aromatic hydrocarbons; The biochemical process processing time is oversize, and clearance only has 30 ~ 40%.
On the other hand, adsorption/desorption plays critical effect to hydrophobic organic pollutant migration in the environment, conversion, biological effectiveness and final environment ownership, as one of important assigning process, there is significant impact to the environmental behaviour of organic pollution.Attapulgite clay refers to attapulgite to be a kind of natural non-metallic clay mineral of essential mineral composition, is mineralogically under the jurisdiction of sepiolite group.Attapulgite is a kind of excellent adsorbent and filter aid.It has the good characteristics such as voidage is high, specific surface is large, proportion is little, adsorptivity is strong, is therefore widely used in water treatment field.
But rarely have the report of attapulgite for the treatment of polycyclic aromatic hydrocarbon in oil extraction waste water at present, the present inventor is not enough for this, deeply seek with the polycyclic aromatic hydrocarbon in attapulgite removal oil extraction waste water, this case produces therefrom.
Summary of the invention
Technical problem to be solved by this invention is to provide the method for a kind of microwave-organically-modified attapulgite and apply the method for polycyclic aromatic hydrocarbon in this attapulgite process oil extraction waste water, be intended to the application widening attapulgite, attapulgite is carried out microwave and organically-modified, make it for the treatment of oil extraction waste water, deeply seek the optimum experimental condition removing the polycyclic aromatic hydrocarbon in oil extraction waste water with attapulgite, for correlative study provides Data support.
For solving the problems of the technologies described above, technical solution of the present invention is:
A method for microwave-organically-modified attapulgite, comprises the steps:
(1) first attapulgite 20 ~ 30g is placed in the conical flask of 250ml, add the cation Gemini surfactant 12-2-12 of 1 ~ 1.5g, the hydrochloric acid of 20 ~ 30ml, 1mol/L, with 80 ~ 100ml deionized water, seal bottleneck, put into the incubator of 50 ~ 60 DEG C, rotating speed 200rpm is set, react 3 ~ 5 hours;
(2) mixed liquor of step (1) is taken out from incubator, put into micro-wave oven and carry out microwave modification;
(3) mixed liquor of step (2) is passed through Buchner funnel suction filtration, and repeatedly rinse by deionized water, until not containing Br in leacheate
-till;
(4) baking oven clay particle that step (3) leaches being placed in 70 ~ 80 DEG C is dried;
(5) solid that step (4) is dried is activated 1 ~ 2 hour at 100 DEG C;
(6) by the soil sample that step (5) obtains, after mortar and process of sieving, microwave-organically-modified good attapulgite is obtained.
In described step (2), arranging microwave intensity is 300 ~ 500W, and the microwave modification time is 3 ~ 5min.
A kind of method applying described polycyclic aromatic hydrocarbon in the attapulgite process oil extraction waste water of modification, modified attapulgite clay adsorbent is directly rendered in oil extraction waste water and carries out adsorption reaction, input ratio is adsorbent mass is 20 ~ 100mg:10 ~ 20ml with wastewater volume ratio, vibrate a period of time under normal temperature, standing separation, can reach purification object.
The sorption reaction time of described polycyclic aromatic hydrocarbon on attapulgite is 24 ~ 48 hours.
The adsorption reaction Optimal pH of described polycyclic aromatic hydrocarbon on attapulgite is for keeping pH value of waste water, and pH value of waste water is 7 ~ 8.
NaN is added in described course of reaction
3solution is to suppress biological agent.
After adopting such scheme, tool of the present invention has the following advantages:
1) experiment shows, modified attapulgite, organo-functional group structure there occurs obvious change.At wave number 3500 and 1500cm
-1having there is new functional group or functional group's displacement in place, enhances its adsorption property.
2) amount of surfactant, the use amount of attapulgite, the microwave time, pH value of solution, reaction temperature all can have an impact to treatment effect.The amount of surfactant, all there is an optimal value (i.e. flex point) to the influence curve for the treatment of effect in the consumption of attapulgite and microwave time, has crossed this flex point, and adsorption efficiency increases slowly, even declines.Advantages of good adsorption effect under acid pH, the adsorption effect under alkali condition is relatively poor.Favors low temperature is in absorption, and high temperature is conducive to desorption.
3) attapulgite is very abundant at the reserves of China, and because traditional activated carbon of sorbent cost is high and regenerate the reasons such as difficulty, attapulgite becomes a kind of environmental protection, cheap adsorbent by replacing active carbon gradually.
4) use cation Gemini surfactant 12-2-12 to carry out organically-modified to attapulgite, the absorption property of attapulgite can be increased substantially.
In a word, the present invention has widened the application of attapulgite, attapulgite is carried out microwave and organically-modified, makes it for the treatment of oil extraction waste water, deeply seek the optimum experimental condition removing the polycyclic aromatic hydrocarbon in oil extraction waste water with attapulgite, for correlative study provides Data support.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
Disclosed is the method for a kind of microwave-organically-modified attapulgite, its specific embodiment is as follows:
Embodiment 1
1) first attapulgite 20g is placed in the conical flask of 250ml, adds the cation Gemini surfactant 12-2-12 of 1g, the hydrochloric acid of 20ml, 1mol/L, with 80ml deionized water, seal bottleneck, put into the incubator of 60 DEG C, rotating speed 200rpm is set, reacts 3 hours.
2) taken out from incubator by the mixed liquor of step 1), put into micro-wave oven, arranging microwave intensity is 400W, and the time is 3min.
3) by step 2) mixed liquor by Buchner funnel suction filtration, and repeatedly to rinse by deionized water, until not containing Br in leacheate
-till, available AgNO
3solution titration is checked.
4) baking oven solid that step 3) leaches being placed in 80 DEG C is dried.
5) solid that step 4) is dried is activated 1 hour at 100 DEG C.
6) soil sample step 5) obtained, after mortar and process of sieving, obtains microwave-organically-modified good attapulgite.Modification soil sample is carried out the analyses such as FTIR, XRD, TGA, characterize modified character.It is for subsequent use that residue puts into drier.
Embodiment 2
1) first attapulgite 30g is placed in the conical flask of 250ml, adds the cation Gemini surfactant 12-2-12 of 1.5g, the hydrochloric acid of 30ml, 1mol/L, with 100ml deionized water, seal bottleneck, put into the incubator of 60 DEG C, rotating speed 200rpm is set, reacts 5 hours.
2) taken out from incubator by the mixed liquor of step 1), put into micro-wave oven, arranging microwave intensity is 500W, and the time is 4min.
3) by step 2) mixed liquor by Buchner funnel suction filtration, and repeatedly to rinse by deionized water, until not containing Br in leacheate
-till, available AgNO
3solution titration is checked.
4) baking oven solid that step 3) leaches being placed in 75 DEG C is dried.
5) solid that step 4) is dried is activated 2 hours at 100 DEG C.
6) soil sample step 5) obtained, after mortar and process of sieving, obtains microwave-organically-modified good attapulgite.Modification soil sample is carried out the analyses such as FTIR, XRD, TGA, characterize modified character.It is for subsequent use that residue puts into drier.
Embodiment 3
1) first attapulgite 25g is placed in the conical flask of 250ml, adds the cation Gemini surfactant 12-2-12 of 1.2g, the hydrochloric acid of 25ml, 1mol/L, with 90ml deionized water, seal bottleneck, put into the incubator of 50 DEG C, rotating speed 200rpm is set, reacts 4 hours.
2) taken out from incubator by the mixed liquor of step 1), put into micro-wave oven, arranging microwave intensity is 300W, and the time is 5min.
3) by step 2) mixed liquor by Buchner funnel suction filtration, and repeatedly to rinse by deionized water, until not containing Br in leacheate
-till, available AgNO
3solution titration is checked.
4) baking oven solid that step 3) leaches being placed in 70 DEG C is dried.
5) solid that step 4) is dried is activated 1.5 hours at 100 DEG C.
6) soil sample step 5) obtained, after mortar and process of sieving, obtains microwave-organically-modified good attapulgite.Modification soil sample is carried out the analyses such as FTIR, XRD, TGA, characterize modified character.It is for subsequent use that residue puts into drier.
Present invention further teaches a kind of method utilizing polycyclic aromatic hydrocarbon in above-mentioned modified attapulgite process oil extraction waste water, its specific embodiment is as follows:
Embodiment 1
Attapulgite is carried out after modification through above-mentioned steps, carries out the adsorption experiment of batch.Oil extraction waste water takes from Hebei province's NW Hebei, has passed through preliminary water-oil separating.Record naphthalene 129.8mg/L in the former water of waste water, luxuriant and rich with fragrance 10.4mg/L, far beyond the emission limit of a polycyclic aromatic hydrocarbon.Get the glass tube of 25ml, often put into the attapulgite modified of 0.02g in pipe, pour the oil extraction waste water of 10ml into, add the NaN of 200mg/L
3solution is to suppress biological agent.Use rubber stopper seal afterwards.Glass tube is placed in the incubator of 25 DEG C, the tachyphylaxis of 200rpm 24 hours, standing separation afterwards.In order to measure as early as possible, first without leaving standstill, directly glass tube can be taken out, centrifugal 30min(5000rpm in centrifuges), get supernatant, after syringe filters is filtered, with ultraviolet specrophotometer, the polycyclic aromatic hydrocarbon content in filtrate is analyzed.Result shows, naphthalene and luxuriant and rich with fragrance removal efficiency reach 93.5 and 91.7% respectively.
Embodiment 2
Attapulgite is carried out after modification through above-mentioned steps, carries out the adsorption experiment of batch.Oil extraction waste water takes from Shandong Province's Shengli Oil Field, has passed through preliminary water-oil separating.Record the Sino-Philippines 7.4mg/L of the former water of waste water, far exceed luxuriant and rich with fragrance emission limit.Get the glass tube of 25ml, often put into the attapulgite modified of 0.03g in pipe, pour the oil extraction waste water of 10ml into.Add the NaN of 200mg/L
3solution is to suppress biological agent.Use rubber stopper seal afterwards.Glass tube is placed in the incubator of 25 DEG C, the tachyphylaxis of 200rpm 48 hours.Afterwards glass tube is taken out, centrifugal 30min(5000rpm in centrifuges).Get supernatant, after syringe filters is filtered, with ultraviolet specrophotometer, the luxuriant and rich with fragrance content in filtrate is analyzed.Result shows, luxuriant and rich with fragrance removal efficiency reaches 95.1%.
The above is only preferred embodiment of the present invention, not imposes any restrictions technical scope of the present invention, therefore the change in every case done according to claim of the present invention and description or modification, all should belong within scope that patent of the present invention contains.
Claims (6)
1. a method for microwave-organically-modified attapulgite, is characterized in that comprising the steps:
(1) first attapulgite 20 ~ 30g is placed in the conical flask of 250ml, add the cation Gemini surfactant 12-2-12 of 1 ~ 1.5g, the hydrochloric acid of 20 ~ 30ml, 1mol/L, with 80 ~ 100ml deionized water, seal bottleneck, put into the incubator of 50 ~ 60 DEG C, rotating speed 200rpm is set, react 3 ~ 5 hours;
(2) mixed liquor of step (1) is taken out from incubator, put into micro-wave oven and carry out microwave modification;
(3) mixed liquor of step (2) is passed through Buchner funnel suction filtration, and repeatedly rinse by deionized water, until not containing Br in leacheate
-till;
(4) baking oven clay particle that step (3) leaches being placed in 70 ~ 80 DEG C is dried;
(5) solid that step (4) is dried is activated 1 ~ 2 hour at 100 DEG C;
(6) by the soil sample that step (5) obtains, after mortar and process of sieving, microwave-organically-modified good attapulgite is obtained.
2. the method for microwave according to claim 1-organically-modified attapulgite, is characterized in that: in described step (2), and arranging microwave intensity is 300 ~ 500W, and the microwave modification time is 3 ~ 5min.
3. application rights requires the method for polycyclic aromatic hydrocarbon in attapulgite process oil extraction waste water described in 1 or 2, it is characterized in that: modified attapulgite clay adsorbent is directly rendered in oil extraction waste water and carries out adsorption reaction, input ratio is adsorbent mass is 20 ~ 100mg:10 ~ 20ml with wastewater volume ratio, vibrate a period of time under normal temperature, standing separation, can reach purification object.
4. the method for polycyclic aromatic hydrocarbon in process oil extraction waste water according to claim 3, is characterized in that: the sorption reaction time of described polycyclic aromatic hydrocarbon on attapulgite is 24 ~ 48 hours.
5. the method for polycyclic aromatic hydrocarbon in process oil extraction waste water according to claim 3, is characterized in that: the adsorption reaction Optimal pH of described polycyclic aromatic hydrocarbon on attapulgite is for keeping pH value of waste water, and pH value of waste water is 7 ~ 8.
6. the method for polycyclic aromatic hydrocarbon in process oil extraction waste water according to claim 3, is characterized in that: add NaN in described course of reaction
3solution is to suppress biological agent.
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Cited By (6)
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| CN105174278A (en) * | 2015-08-17 | 2015-12-23 | 天津大学 | Preparation method for modified attapulgite, and method for preparing soil conditioner with attapulgite as main raw material |
| CN105233570A (en) * | 2015-10-27 | 2016-01-13 | 广东工业大学 | Novel metal oxide iron-copper composite modified quartz sand filter material, and preparation method and application thereof |
| CN106118680A (en) * | 2016-06-28 | 2016-11-16 | 安徽金联地矿科技有限公司 | A kind of preparation method of contaminated soil remediation material based on attapulgite |
| CN106591279A (en) * | 2017-02-08 | 2017-04-26 | 光合强化（北京）生物科技有限公司 | Modified attapulgite used for immobilizing polycyclic aromatic hydrocarbon degrading bacteria, and preparation method thereof |
| CN109985443A (en) * | 2019-04-02 | 2019-07-09 | 周振坤 | A kind of air purifier |
| CN111732156A (en) * | 2020-07-29 | 2020-10-02 | 东北农业大学 | Method for inhibiting release of polycyclic aromatic hydrocarbons in rice and crab co-culture paddy field sediment polluted by medium and light polycyclic aromatic hydrocarbons |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174278A (en) * | 2015-08-17 | 2015-12-23 | 天津大学 | Preparation method for modified attapulgite, and method for preparing soil conditioner with attapulgite as main raw material |
| CN105233570A (en) * | 2015-10-27 | 2016-01-13 | 广东工业大学 | Novel metal oxide iron-copper composite modified quartz sand filter material, and preparation method and application thereof |
| CN105233570B (en) * | 2015-10-27 | 2017-12-26 | 广东工业大学 | A kind of composite modified quartz sand filter media of metal oxide iron copper and its preparation method and application |
| CN106118680A (en) * | 2016-06-28 | 2016-11-16 | 安徽金联地矿科技有限公司 | A kind of preparation method of contaminated soil remediation material based on attapulgite |
| CN106591279A (en) * | 2017-02-08 | 2017-04-26 | 光合强化（北京）生物科技有限公司 | Modified attapulgite used for immobilizing polycyclic aromatic hydrocarbon degrading bacteria, and preparation method thereof |
| CN109985443A (en) * | 2019-04-02 | 2019-07-09 | 周振坤 | A kind of air purifier |
| CN111732156A (en) * | 2020-07-29 | 2020-10-02 | 东北农业大学 | Method for inhibiting release of polycyclic aromatic hydrocarbons in rice and crab co-culture paddy field sediment polluted by medium and light polycyclic aromatic hydrocarbons |
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