CN110272090A - A kind of method of multifunction magnetic hydrogel processing waste water - Google Patents
A kind of method of multifunction magnetic hydrogel processing waste water Download PDFInfo
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- CN110272090A CN110272090A CN201910306551.3A CN201910306551A CN110272090A CN 110272090 A CN110272090 A CN 110272090A CN 201910306551 A CN201910306551 A CN 201910306551A CN 110272090 A CN110272090 A CN 110272090A
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- magnetic hydrogel
- multifunction magnetic
- waste water
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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
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The present invention relates to a kind of methods with multifunction magnetic hydrogel processing waste water.System is caused using Nanoscale Iron/hydrogen peroxide, polyethyleneglycol diacrylate and initiator are mixed into solvent, it is sealed after being passed through nitrogen deoxygenation, controls reaction temperature at 28 DEG C, react 2 hours, products therefrom is after eluting solvent sufficiently washs, under only with gravity, separated for oil hydrosol, water-oil separating efficiency is up to 99.6%, the multifunction magnetic hydrogel of preparation can also be used for the degradation of methylene blue, and degradation rate is up to 99.5%.Preparation method of the present invention is simple and reliable, and post-processing is simple, and resulting materials recycling rate of waterused is good.Initiator Fe in initiation system3O4NPs uniformly and quantitatively disperses in the material after causing polymerization, and still maintains catalytic performance, Fe after polymerizeing3O4The magnetism of NPs makes it easier to recycle, degradation of the obtained magnetic hydrogel for the quick separating and organic dyestuff in wastewater of oil hydrosol.
Description
Technical field
The present invention relates to multifunction magnetic hydrogel answering in terms of oil hydrosol separation and organic dyestuff in wastewater degradation
With belonging to technical field of waste water processing.
Background technique
Water is Source of life, is the material base of human survival.Oily waste water is ubiquitous, derived from industrial production and daily
Life, brings grave danger to the sustainable development and human health in the world.Therefore, it is to utilize water that oily waste water, which is effectively treated,
The necessary means of resource, this is also a problem to be solved.In oily waste water, since emulsion droplet is by surfactant packet
It covers, keeps lotion more stable, which increase isolated difficulty, therefore water-oil separating is the key that processing oily waste water.Conventional oil
Water separating method has gravitational method, centrifugal process, absorption method, floatation, chemical method etc..In general, the oil-in-water that surfactant is stable
The separation of lotion usually requires multistep process, and the technique including a variety of method collaborations such as demulsification-coagulation/air bearing/absorption-separation is
It is able to achieve, there is the defects of with duration and low separation efficiency.In recent years, the net materials with special wetting property are applied to water oil
The separation of lotion.These net materials have super-hydrophobic, underwater superoleophobic special Wettability under super hydrophilic super oleophylic, oil.Example
Such as: Chinese patent document CN106215462A discloses a kind of based on the super-hydrophobic/super close of POSS base hydridization acrylate coatings
Oily stainless (steel) wire and the preparation method and application thereof, resulting materials can have super-hydrophobic/super-oleophilic, can be applied to industrial grease
The separation of mixture.Chinese patent document CN109603208A discloses a kind of net and preparation method thereof for water-oil separating,
Resulting materials have super hydrophilic while underwater superoleophobic surface, can be applied to water-oil separating.However, easy to pollute and recycling rate of waterused
Low disadvantage limits the practical ranges of net materials.Therefore, preparation is simple, separation is efficient, high recycling rate material
With bigger practical significance.
Methylene blue is water-soluble polycyclic aromatic hydrocarbon dyestuff.Currently, methylene blue is widely used in chemical engineering industry and weaving print
Dyer's industry.Waste water largely containing methylene blue dye can be generated in industrial processes, waste water has serious toxicity and harm,
A regional water quality will be directly affected, ambient enviroment is destroyed and is detrimental to health.Since structure is complicated for methylene blue, waste water
With high concentration, the characteristics of high chroma and high ph-values, therefore, it is difficult to handle.Processing method reported at present is divided into three categories:
Advanced oxidation processes (AOP), biodegrade processing and absorption.Fenton's reaction belongs to chemical oxidation of gold, due to excellent degradation
Rate and degradation are easy to operate, become one of processing organic wastewater most efficient method.Traditional homogeneous Fenton's reaction tool
There is higher catalytic activity, but there are disadvantages for the reaction, such as difficult separation, the rate of recovery is low, at high cost.In recent years, there is high stable
The detachable magnetic Fenton-type catalysts of property cause extensive attention.Such as Fe3O4 NPs/H2O2Redox system, the body
System has been widely used for degradating organic dye, and magnetic nano-particle is easily isolated under the intervention of external magnetic field.However, receiving
The small and easy to reunite characteristic of rice grain partial size is difficult to recycle in actual use so that its catalytic activity reduces, and increases life
Produce cost.Therefore, a kind of material being easily recycled and have high degradation efficiency, is more suitable for actual production.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of multifunctional material to solve above-mentioned ask
Topic.The present invention uses the multifunctional water gel with magnetic, particular interface wettability and efficient catalytic degrading activity to carry out oil
The degradation of aqueous emulsion separation and organic dyestuff.The polymer is that have hydrophilic monomer by introducing, and is aided with unique
The nano particle of energy, takes water as a solvent, is prepared by nanoparticle mediated free radical polymerization, has super close in air
Super oleophylic in water, air, under oil super hydrophilic, underwater oleophobic infiltration feature, can realize oil hydrosol only under the effect of gravity
Separation.Material has efficient catalytic activity simultaneously, can cooperate degradating organic dye with hydrogen peroxide.
The scheme of the invention is:
A kind of multifunction magnetic hydrogel oil-water separation lotion, the method for degradating organic dye, steps are as follows:
After multifunction magnetic hydrogel is added water-swellable balance, oil hydrosol to be separated is added, relies on gravity, to grease
Lotion is separated;
It after multifunction magnetic hydrogel is added hydrogen peroxide swelling equilibrium, puts into methylene blue dye solution, stands, complete sub-
The degradation of methyl blue dye;
The multifunction magnetic hydrogel is prepared as follows to obtain:
Hydrophilic monomer polyethyleneglycol diacrylate, nano ferriferrous oxide granule are added in solvent and are mixed, body is adjusted
The pH value of system after being passed through nitrogen deoxygenation, is added hydrogen peroxide sealing, is stored at room temperature, react 2 seconds ~ 4 hours, and product is molten through eluting
After agent is sufficiently washed, it is freeze-dried to get multifunction magnetic hydrogel.
, according to the invention it is preferred to, the mass ratio of the polyethyleneglycol diacrylate and nano ferriferrous oxide is
1:(0.01 ~ 0.5), further preferred 1:(0.05 ~ 0.2).
, according to the invention it is preferred to, the number-average molecular weight of the polyethyleneglycol diacrylate is 575-700, described
Nano ferriferrous oxide average grain diameter be 20nm.
, according to the invention it is preferred to, the initiator be the oxidation of nano ferriferrous oxide and hydrogen peroxide composition also
Former initiation system;
Preferably, the solvent is the combination of one or both of water and hydrochloric acid;
Preferably, the initiator accounts for the weight percent of polyethyleneglycol diacrylate between 2 ~ 40%;
Preferably, the eluting solvent is ethyl alcohol;
Preferably, the system pH is between 1~7.
, according to the invention it is preferred to, the room temperature is between 25 DEG C ± 3 DEG C;Reaction time was at 2 seconds ~ 4 hours.
According to the present invention, the oil hydrosol refers to the oil hydrosol or living containing surface not comprising surfactant
The oil hydrosol of property agent (such as Tween 80).The organic dyestuff refers to that methylene blue is dissolved in aqueous solution after adjusting pH
Methylene blue dye solution.
The separation method of oil hydrosol according to the present invention, a kind of preferred embodiment are as follows:
Multifunction magnetic hydrogel is placed in column shape container, after adding water-swellable balance, grease cream is added from column shape container top
Liquid relies on gravity, and oil hydrosol flows through polymer material, and oil hydrosol is demulsified when flowing through column material, and water can be suitable
Benefit is but retained by polymer material, oil in the polymeric material, to realize the separation of oil hydrosol.
According to the present invention, multifunction magnetic hydrogel material can reuse after ethyl alcohol sufficiently washs.Make repeatedly
With 7 times or more, water-oil separating efficiency is maintained at 95.8% or more.
The processing method of methylene blue dye wastewater according to the present invention, a kind of preferred embodiment are as follows:
After multifunction magnetic hydrogel is added hydrogen peroxide swelling equilibrium, put into methylene blue dye solution, it is static, it completes sub-
The degradation of methyl blue.Degradation rate is up to 99.5%.
According to the present invention, the preparation of the multifunction magnetic hydrogel, a kind of preferred embodiment are as follows:
The polyethyleneglycol diacrylate of 0.4 mL is taken, 22 mg nano ferriferrous oxide granules are added to 1.59 mL's
It is mixed in aqueous solution, the pH of regulation system is 2.5.After being passed through nitrogen deoxygenation, sealed after 10 μ L hydrogen peroxide are added, at room temperature
It stands, reacts 2 hours;For products therefrom after eluting solvent sufficiently washs, freeze-drying obtains multifunction magnetic hydrogel.
The features of the present invention and beneficial effect are:
Multifunction magnetic hydrogel material of the invention has advantage environmentally protective, rapidly and efficiently, while having in air
The property of super hydrophilic, underwater oleophobic under super hydrophilic super oleophylic, oil, suitable for the separation of oil hydrosol, separation process only needs gravity
Effect is i.e. implementable, is not necessarily to impressed pressure device, and water-oil separating efficiency is higher than 99.3%, which is suitable for organic dyestuff simultaneously
Degradation, 99.5% is up to the degradation rate of methylene blue.Preparation method of the present invention is simple and reliable, and post-processing is simple, resulting materials
Recycling rate of waterused is good.Degradation of the obtained magnetic hydrogel for the quick separating and organic dyestuff in wastewater of oil hydrosol.
Detailed description of the invention
Fig. 1: separation process of the multifunction magnetic hydrogel to oil hydrosol made from embodiment 1.
Fig. 2: the repeat performance that multifunction magnetic hydrogel separates oil hydrosol made from embodiment 1.
Fig. 3: degradation and separation process of the multifunction magnetic hydrogel made from embodiment 1 to methylene blue dye wastewater.
Specific embodiment
Below by specific embodiment and in conjunction with attached drawing, the invention will be further described, but not limited to this.
Embodiment 1
The polyethyleneglycol diacrylate of 0.4 mL is taken, 22 mg nano ferriferrous oxide granules are added to 1.59 mL's
It is mixed in aqueous solution, the pH of regulation system is 2.5.After being passed through nitrogen deoxygenation, sealed after 10 μ L hydrogen peroxide are added, at room temperature
It stands, reacts 2 hours;For products therefrom after eluting solvent sufficiently washs, freeze-drying obtains multifunction magnetic hydrogel;
The oil hydrosol separation process schematic diagram of multifunction magnetic hydrogel made from the present embodiment is as shown in Figure 1;
Gained magnetic hydrogel is placed in syringe, adds water-swellable balance after 2 hours, 2 mL greases are added from column tube top
Lotion, only with gravity, oil hydrosol can flow through polymer column material, and water passes through material, and oil is retained in material
In material, filtrate clarification, water-oil separating efficiency is 99.6%.Polymer material after ethyl alcohol sufficiently washs, Reusability 7 times with
On, water-oil separating efficiency is not less than 95.8%(Fig. 2).
Embodiment 2
44 mg nano ferriferrous oxide granules are taken, is added in the aqueous solution of 1.59 mL and mixes, the pH of regulation system is
2.5, the polyethyleneglycol diacrylate of 0.4 mL is added.It is passed through nitrogen deoxygenation, is sealed after 20 μ L hydrogen peroxide are added after concussion,
Constant temperature is stood at 28 DEG C, is reacted 2 hours;For products therefrom after eluting solvent sufficiently washs, freeze-drying obtains multi-function magnetic
Property hydrogel;
Gained magnetic hydrogel is placed in syringe, adds water-swellable balance after 2 hours, 2 mL greases are added from column tube top
Lotion, only with gravity, oil hydrosol can flow through polymer column material, and water passes through material, and oil is retained in material
In material, water-oil separating efficiency is 99.4%.
Embodiment 3
The polyethyleneglycol diacrylate of 0.4 mL is taken, 22 mg nano ferriferrous oxide granules are added to the water of 1.59 mL
It is mixed in solution, the pH of regulation system is 2.5.After being passed through nitrogen deoxygenation, sealed after 10 μ L hydrogen peroxide are added, it is quiet at room temperature
It sets, reacts 2 hours;For products therefrom after eluting solvent sufficiently washs, freeze-drying obtains multifunction magnetic hydrogel;
Multifunction magnetic hydrogel is placed in vial, after adding hydrogen peroxide swelling equilibrium 2 hours, the Asia of 80 mg/L is added
The degradation of organic dyestuff, degradation rate 99.5% can be realized in methyl blue dye;
Degradation process schematic diagram such as Fig. 3 institute of the methylene blue dye wastewater of multifunction magnetic hydrogel made from the present embodiment
Show.
Claims (10)
1. a kind of multifunction magnetic hydrogel oil-water separation lotion, the method for degradation of methylene blue dye solution, steps are as follows:
After multifunction magnetic hydrogel is added water-swellable balance, oil hydrosol to be separated is added, relies on gravity, to grease
Lotion is separated;
It after multifunction magnetic hydrogel is added hydrogen peroxide swelling equilibrium, puts into methylene blue dye solution, stands, complete sub-
The degradation of methyl blue dye;
The multifunction magnetic hydrogel is prepared as follows to obtain:
Hydrophilic monomer polyethyleneglycol diacrylate, nano ferriferrous oxide granule are added in solvent and are mixed, nitrogen is passed through
After gas deoxygenation, hydrogen peroxide sealing is added, is placed at room temperature for, reacts 2 seconds ~ 4 hours, product is cold after eluting solvent sufficiently washs
It is lyophilized dry to get multifunction magnetic hydrogel.
2. as described in claim 1 with the method for multifunction magnetic hydrogel processing waste water, it is characterised in that the poly- second
The mass ratio of omega-diol diacrylate and nano ferriferrous oxide is 1:(0.01 ~ 0.5), further preferred 1:(0.05 ~ 0.2).
3. as described in claim 1 with the method for multifunction magnetic hydrogel processing waste water, it is characterised in that the poly- second
The number-average molecular weight of omega-diol diacrylate is 575-700, and the average grain diameter of the nano ferriferrous oxide is 20nm.
4. as described in claim 1 with the method for multifunction magnetic hydrogel processing waste water, it is characterised in that the initiation
Agent is the redox initiation system of nano ferriferrous oxide and hydrogen peroxide composition.
5. as described in claim 1 with the method for multifunction magnetic hydrogel processing waste water, it is characterised in that the solvent
It is the combination of one or both of water and hydrochloric acid.
6. as described in claim 1 with the method for multifunction magnetic hydrogel processing waste water, it is characterised in that the initiation
Agent accounts for the weight percent of polyethyleneglycol diacrylate between 2 ~ 40%.
7. as described in claim 1 with the method for multifunction magnetic hydrogel processing waste water, it is characterised in that the elution
Solvent is ethyl alcohol.
8. as described in claim 1 with the method for multifunction magnetic hydrogel processing waste water, it is characterised in that the reaction
25 ± 3 DEG C of temperature;Reaction time was at 2 seconds ~ 4 hours.
9. as described in claim 1 with the method for multifunction magnetic hydrogel processing waste water, it is characterised in that oil hydrosol point
It is comprised the following steps that from organic dyestuff in wastewater degradation
Multifunction magnetic hydrogel is placed in column shape container, after adding water-swellable balance, grease cream is added from column shape container top
Liquid relies on gravity, and oil hydrosol flows through polymer material, and oil hydrosol is demulsified when flowing through column material, and water can be suitable
Benefit is but retained by polymer material, oil in the polymeric material, to realize the separation of oil hydrosol;
After multifunction magnetic hydrogel is added hydrogen peroxide swelling equilibrium, put into methylene blue dye solution, it is static, it completes sub-
The degradation of methyl blue.
10. as described in claim 1 with the method for multifunction magnetic hydrogel processing waste water, it is characterised in that more function
The preparation step of energy magnetic hydrogel is as follows:
The polyethyleneglycol diacrylate of 0.4 mL is taken, 22 mg nano ferriferrous oxide granules are added to the water of 1.59 mL
It is mixed in solution, the pH of regulation system is 2.5;
It after being passed through nitrogen deoxygenation, seals after 10 μ L hydrogen peroxide are added, stands at room temperature, react 2 hours, products therefrom is through washing
After desolventizing sufficiently washs, freeze-drying obtains multifunction magnetic hydrogel.
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CN112591848A (en) * | 2020-12-23 | 2021-04-02 | 清华海峡研究院(厦门) | Oil-water separation method and system for oily sewage |
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EP1795211A2 (en) * | 1998-03-03 | 2007-06-13 | Nippon Shokubai Co., Ltd. | Water-absorbing agent and its production process and use |
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