CN106944019A - A kind of adsorption stuffing of processing containing aniline waste water and its production and use - Google Patents
A kind of adsorption stuffing of processing containing aniline waste water and its production and use Download PDFInfo
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- C02F1/00—Treatment of water, waste water, or sewage
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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Abstract
The invention belongs to technical field of waste water processing, it is related to a kind of adsorption stuffing of processing containing aniline waste water and its production and use.Specifically, preparation method of the invention includes：1) surfactant and the mixed solution of water as aqueous phase are prepared；2) mixed solution of the acrylate, styrene and aminostyryl as oil phase is prepared；3) O/W type emulsions are prepared；4) free-radical emulsion polymerization, preparation method is simple and easy to do.The particle diameter of the adsorption stuffing prepared by this method is 200~2000 μm, can effectively adsorb and be enriched with the aniline in water, and easily zeolite regeneration, it is adaptable to the industrial treatment containing aniline waste water.
Description
Technical field
The invention belongs to technical field of waste water processing, it is related to a kind of adsorption stuffing of the processing containing aniline waste water, its preparation side
Method, and its purposes in being handled containing aniline waste water.
Background technology
Aniline is most representational aromatic amine material, is a kind of colourless oil liquid with aromatic odor, extensively
Applied to industries such as national defence, printing and dyeing, plastics, paint, agricultural chemicals and medicine.In addition, aniline is also a kind of severe contamination environment and danger
The harmful substance of evil health, belong to " carcinogenic, teratogenesis, mutagenesis " three cause material.Due to aniline have extended residual,
The features such as bioconcentration, carcinogenicity, 129 kinds of pollutants of priority acccess control are classified as by U.S. EPA；Meanwhile, its be also put into " in
In state's priority pollutant blacklist ", strict control is required in industrial water drainage.The method of processing amino benzene analog waste water mainly has
The methods such as physics, chemistry, biology, specific such as extraction, photocatalytic oxidation, sonication.
The Chinese invention patent application of Application No. 201410593332.5 discloses a kind of processing side of amino benzene analog waste water
Method, is combined through polycondensation reaction-Fenton-NaClO oxidation technologies, significantly reduces the COD and aniline content of amino benzene analog waste water, and
This method is produced without solid waste, will not cause secondary pollution.But, because the process step of this method is relatively complicated, be related to heating,
The steps such as pH value, flocculation are adjusted, therefore are not suitable for the processing of high-volume industrial wastewater；Application No. 201610095154.2
Chinese invention patent application discloses a kind of method that amino benzene analog waste water is handled by mushroom edman degradation Edman, each strain of this method it
Between symbiosis coordinate, mutually not antagonism, is added in Waste Water Treatment, has good degraded effect to phenyl amines difficult degradation compound
Really.But, mushroom regeneration is more numerous and diverse, is not also suitable for the processing of high-volume industrial wastewater.
The content of the invention
For there is no effectively this present situation of processing method of the high-volume containing aniline waste water at present, the present invention is intended to provide a kind of
Adsorption stuffing containing aniline waste water and preparation method thereof is handled, the adsorption stuffing prepared by this method has to the aniline in waste water
There are obviously concentration effect, and easily zeolite regeneration, it is adaptable to the in high volume processing containing aniline waste water.
Specifically, the present invention is adopted the following technical scheme that：
A kind of preparation method for handling the adsorption stuffing containing aniline waste water, it comprises the following steps：
1) surfactant and the mixed solution of water as aqueous phase are prepared：
At ambient temperature, nonionic surface active agent, anionic surfactant and water are stirred, obtained
The mixed solution of surfactant and water；
2) mixed solution of the acrylate, styrene and aminostyryl as oil phase is prepared：
At ambient temperature, acrylate, styrene and aminostyryl are stirred, obtains acrylate, benzene second
The mixed solution of alkene and aminostyryl；
3) O/W type emulsions are prepared：
At ambient temperature, to step 2) in the obtained mixed solution of acrylate, styrene and aminostyryl
Add radical initiator, after stirring and dissolving, be then added to step 1) in obtained surfactant and water mixed solution in,
Shear agitation, until obtaining O/W type emulsions；
4) free-radical emulsion polymerization：
By step 3) in obtained O/W types emulsion heating, initiated polymerization, after reaction terminates, through filtering, washing and true
Sky is dried, and obtains handling the adsorption stuffing containing aniline waste water.
In a preferred embodiment, step 1) described in nonionic surface active agent be selected from Tween-20, tell
Temperature -80, Qula lead to X-65, and triton x-100, Qula lead to any one in X-165 and modified cellulose, preferably Tween-20
Or Qula leads to X-65；The anionic surfactant is dodecyl sodium sulfate or neopelex, preferably ten
Dialkyl sulfonates；The water is deionized water, and its resistivity is more than 18.2M Ω.
In a preferred embodiment, step 1) described in surfactant and water mixed solution in surface-active
The mass concentration of agent is 5~20g/L, preferably 14g/L, and the nonionic surface active agent accounts for surfactant gross mass
85%~95%, preferably 90%~93%.
In a preferred embodiment, step 2) described in acrylate be selected from methyl acrylate, ethyl acrylate
With any one in butyl acrylate, preferably methyl acrylate；The aminostyryl is 3- aminostyryls or 4- amino
Styrene, preferably 4- aminostyryls.
In a preferred embodiment, step 2) described in acrylate, styrene and aminostyryl quality
Than for 5~10:1~3:1~3, preferably 8:1:1.
In a preferred embodiment, step 3) described in radical initiator be azo type free radical initiator or
Peroxy type free radical initiator, the wherein preferred azodiisobutyronitrile of azo type free radical initiator, peroxy type free radical initiator
It is preferred that benzoyl peroxide.
In a preferred embodiment, step 3) described in acrylate, styrene and aminostyryl mixing
The mass ratio of solution and radical initiator is 100:0.1~0.5, preferably 100:0.2.
In a preferred embodiment, step 3) described in the speed of agitator of shear agitation be 50~800 revs/min
Clock, preferably 80~500 revs/min.
In a preferred embodiment, step 3) described in O/W type emulsions oil phase drop particle diameter for 200~
2000 μm, preferably 300~1000 μm.
In a preferred embodiment, step 4) described in the target temperature that heats up be 40~80 DEG C, preferably 50~
70℃。
In a preferred embodiment, step 4) described in filter and completed using filter membrane or filter paper, wherein filter membrane
It is preferred that aperture is 20 μm of nylon leaching film, the preferred aperture of filter paper is 5 μm of aqueous filter paper.
In a preferred embodiment, step 4) described in wash Shui Hejia successively using 0.5 times of original volume
Alcohol is completed, wherein washing 1 time, alcohol washes 4 times；The used preferred deionized water of water, the used preferred chromatographically pure first of methanol
Alcohol.
In a preferred embodiment, step 4) described in vacuum drying vacuum be 15kPa, drying temperature is
78 DEG C, drying time is 20 hours.
A kind of adsorption stuffing of the processing containing aniline waste water, it is made by above-mentioned preparation method.
In a preferred embodiment, the particle diameter of the adsorption stuffing of the processing containing aniline waste water is 200~2000 μ
m。
Purposes of adsorption stuffing of the above-mentioned processing containing aniline waste water in being handled containing aniline waste water.
Experiment is proved：Adsorption stuffing of the processing containing aniline waste water of the present invention can effectively adsorb and be enriched with the benzene in water
Amine, and easily zeolite regeneration, preparation method are simple and easy to do, it is adaptable to the industrial treatment containing aniline waste water.
Brief description of the drawings
Fig. 1 is the HPLC spectrograms of 100ppm aniline-water solutions.
Fig. 2 is the HPLC spectrograms of efflux after 86 times of column volumes of loading.
Fig. 3 is the HPLC spectrograms of efflux after 87 times of column volumes of loading.
Fig. 4 is the HPLC spectrograms of efflux after upper 5 column volumes of eluant, eluent.
Embodiment
Further elucidated above is made to the technical scheme in the present invention below in conjunction with the drawings and specific embodiments.Unless another
It is described, instrument, reagent, material used in the following example etc. can be obtained by routine business means.
Embodiment 1：Handle the preparation of the adsorption stuffing containing aniline waste water.
At room temperature, deionized water (500mL), triton x-100 (6.3g) and dodecyl sodium sulfate (0.7g) are added
Enter into 1L three-necked bottles, stir 30min, obtain uniform aqueous phase solution.
At room temperature, methyl acrylate (80g), styrene (10g) and 4- aminostyryls (10g) are added to 500mL
In conical flask, stir, obtain the oil-phase solution of water white transparency.
At room temperature, add after azodiisobutyronitrile (0.2g), stirring and dissolving, be then added into above-mentioned oil-phase solution
State in aqueous phase solution, (domestic S312-90 mechanical agitators, the tactical diameter of stirring sheet is 10cm to shear agitation, and speed of agitator is
500rpm), until obtaining uniform and stable O/W types emulsion (average grain diameter of oil phase drop is about 300 μm).
Above-mentioned emulsion is warming up to 60 DEG C, initiated polymerization reacts after 10h, 30 DEG C is cooled to, with 20 μm of nylon leaching films
Filtering, filter cake is washed 1 time with the deionized water of 0.5 times of original volume, then is washed with the methanol (chromatographically pure) of 0.5 times of original volume
Wash 4 times, then filter cake is transferred in stainless steel pallet, (15kPa) 20h is dried in vacuo in 78 DEG C, obtain white and (show slightly sometimes
It is light yellow) powdered absorption filler (69g), average grain diameter is about 300 μm.
Embodiment 2：Handle the preparation of the adsorption stuffing containing aniline waste water.
At room temperature, deionized water (500mL), Tween-20 (6.5g) and neopelex (0.5g) are added
Into 1L three-necked bottles, 30min is stirred, uniform aqueous phase solution is obtained.
At room temperature, ethyl acrylate (80g), styrene (10g) and 3- aminostyryls (10g) are added to 500mL
In conical flask, stir, obtain the oil-phase solution of water white transparency.
At room temperature, add after azodiisobutyronitrile (0.2g), stirring and dissolving, be then added into above-mentioned oil-phase solution
State in aqueous phase solution, (domestic S312-90 mechanical agitators, the tactical diameter of stirring sheet is 10cm to shear agitation, and speed of agitator is
300rpm), until obtaining uniform and stable O/W types emulsion (average grain diameter of oil phase drop is about 500 μm).
Above-mentioned emulsion is warming up to 70 DEG C, initiated polymerization reacts after 10h, 30 DEG C is cooled to, with 20 μm of nylon leaching films
Filtering, filter cake is washed 1 time with the deionized water of 0.5 times of original volume, then is washed with the methanol (chromatographically pure) of 0.5 times of original volume
Wash 4 times, then filter cake is transferred in stainless steel pallet, (15kPa) 20h is dried in vacuo in 78 DEG C, obtain white and (show slightly sometimes
It is light yellow) powdered absorption filler (76g), average grain diameter is about 500 μm.
Embodiment 3：Handle the preparation of the adsorption stuffing containing aniline waste water.
At room temperature, deionized water (500mL), Tween-20 (6.5g) and neopelex (0.5g) are added
Into 1L three-necked bottles, 30min is stirred, uniform aqueous phase solution is obtained.
At room temperature, butyl acrylate (50g), styrene (30g) and 4- aminostyryls (20g) are added to 500mL
In conical flask, stir, obtain the oil-phase solution of water white transparency.
At room temperature, add after azodiisobutyronitrile (0.2g), stirring and dissolving, be then added into above-mentioned oil-phase solution
State in aqueous phase solution, (domestic S312-90 mechanical agitators, the tactical diameter of stirring sheet is 10cm to shear agitation, and speed of agitator is
80rpm), until obtaining uniform and stable O/W types emulsion (average grain diameter of oil phase drop is about 1000 μm).
Above-mentioned emulsion is warming up to 70 DEG C, initiated polymerization reacts after 10h, 30 DEG C is cooled to, with 20 μm of nylon leaching films
Filtering, filter cake is washed 1 time with the deionized water of 0.5 times of original volume, then is washed with the methanol (chromatographically pure) of 0.5 times of original volume
Wash 4 times, then filter cake is transferred in stainless steel pallet, (15kPa) 20h is dried in vacuo in 78 DEG C, obtain white and (show slightly sometimes
It is light yellow) powdered absorption filler (77g), average grain diameter is about 1000 μm.
Embodiment 4：Handle the preparation of the adsorption stuffing containing aniline waste water.
At room temperature, deionized water (500mL), Tween-20 (6.5g) and neopelex (0.5g) are added
Into 1L three-necked bottles, 30min is stirred, uniform aqueous phase solution is obtained.
At room temperature, methyl acrylate (80g), styrene (10g) and 4- aminostyryls (10g) are added to 500mL
In conical flask, stir, obtain the oil-phase solution of water white transparency.
At room temperature, add after benzoyl peroxide (0.2g), stirring and dissolving, be then added into above-mentioned oil-phase solution
State in aqueous phase solution, (domestic S312-90 mechanical agitators, the tactical diameter of stirring sheet is 10cm to shear agitation, and speed of agitator is
100rpm), until obtaining uniform and stable O/W types emulsion (average grain diameter of oil phase drop is about 800 μm).
Above-mentioned emulsion is warming up to 50 DEG C, initiated polymerization reacts after 20h, 30 DEG C is cooled to, with 20 μm of nylon leaching films
Filtering, filter cake is washed 1 time with the deionized water of 0.5 times of original volume, then is washed with the methanol (chromatographically pure) of 0.5 times of original volume
Wash 4 times, then filter cake is transferred in stainless steel pallet, (15kPa) 20h is dried in vacuo in 78 DEG C, obtain white and (show slightly sometimes
It is light yellow) powdered absorption filler (87g), average grain diameter is about 800 μm.
Embodiment 5：Contain aniline waste water using the adsorption stuffing processing of the present invention.
10g particle diameters are arrived for 200 μm of adsorption stuffing dry packIn chromatographic column, 100ppm benzene is prepared
Amine aqueous solution.The aniline-water solution is pumped into chromatographic column with 1mL/min flow velocity, until can in the efflux of chromatographic column lower end
Untill detecting aniline.Then the ethanol as eluant, eluent is pumped into chromatographic column, until in the efflux of chromatographic column lower end no longer
Untill being able to detect that aniline.Aniline content in efflux is determined by HPLC, as a result shown：Aniline content in efflux
For 95 times of aniline-water solution, the aniline in water can effectively be adsorbed by illustrating the adsorption stuffing of the present invention.It is further used as elution
The ethanol/water (75 of agent:25v/v) elute after 6 column volumes, no longer detect aniline in elution efflux, illustrate the present invention's
Adsorption stuffing easily regenerates.
Embodiment 6：Contain aniline waste water using the adsorption stuffing processing of the present invention.
10g particle diameters are arrived for 800 μm of adsorption stuffing dry packIn chromatographic column, 100ppm benzene is prepared
Amine aqueous solution, and record its HPLC collection of illustrative plates (as shown in Figure 1).The aniline-water solution is pumped into chromatographic column with 1mL/min flow velocity
In, untill aniline is able to detect that in the efflux of chromatographic column lower end.Then the ethanol as eluant, eluent is pumped into chromatographic column
In, untill being no longer able to detect aniline in the efflux of chromatographic column lower end.The aniline in efflux is determined by HPLC to contain
Amount, as a result shows：Aniline content in efflux is 87 times of aniline-water solution, illustrates that the adsorption stuffing of the present invention can be effective
Aniline in ground absorption water.It is further used as the ethanol/water (65 for eluant, eluent:35) elute after 5 column volumes, in elution efflux not
Aniline is detected again, illustrates that the adsorption stuffing of the present invention easily regenerates (as shown in Figures 2 to 4).
Embodiment 7：Contain aniline waste water using the adsorption stuffing processing of the present invention.
10g particle diameters are arrived for 1500 μm of adsorption stuffing dry packIn chromatographic column, 100ppm benzene is prepared
Amine aqueous solution.The aniline-water solution is pumped into chromatographic column with 1mL/min flow velocity, until can in the efflux of chromatographic column lower end
Untill detecting aniline.Then the ethanol as eluant, eluent is pumped into chromatographic column again, until in the efflux of chromatographic column lower end not
Untill being able to detect that aniline again.Aniline content in efflux is determined by HPLC, as a result shown：Aniline in efflux contains
Measure as 73 times of aniline-water solution, the aniline in water can effectively be adsorbed by illustrating the adsorption stuffing of the present invention.It is further used as washing
The ethanol/water (55 of de- agent:45) elute after 3 column volumes, no longer detect aniline in elution efflux, illustrate the suction of the present invention
Attached filler easily regenerates.
Claims (10)
1. a kind of preparation method for handling the adsorption stuffing containing aniline waste water, it is characterised in that：
The preparation method comprises the following steps：
1) surfactant and the mixed solution of water as aqueous phase are prepared：
At ambient temperature, nonionic surface active agent, anionic surfactant and water are stirred, obtains surface
The mixed solution of activating agent and water；
2) mixed solution of the acrylate, styrene and aminostyryl as oil phase is prepared：
At ambient temperature, acrylate, styrene and aminostyryl are stirred, obtain acrylate, styrene and
The mixed solution of aminostyryl；
3) O/W type emulsions are prepared：
At ambient temperature, to step 2) in add in the obtained mixed solution of acrylate, styrene and aminostyryl
After radical initiator, stirring and dissolving, be then added to step 1) in obtained surfactant and water mixed solution in, shearing
Stirring, until obtaining O/W type emulsions；
4) free-radical emulsion polymerization：
By step 3) in obtained O/W types emulsion heating, initiated polymerization is dry through filtering, washing and vacuum after reaction terminates
It is dry, obtain handling the adsorption stuffing containing aniline waste water.
2. preparation method according to claim 1, it is characterised in that：
Step 1) described in nonionic surface active agent be selected from Tween-20, Tween-80, Qula lead to X-65, triton x-100,
Qula leads to any one in X-165 and modified cellulose；The anionic surfactant be dodecyl sodium sulfate or
Neopelex；The water is deionized water.
3. preparation method according to claim 1, it is characterised in that：
Step 1) described in surfactant and water mixed solution in surfactant mass concentration be 5~20g/L, and
The nonionic surface active agent accounts for the 85%~95% of surfactant gross mass.
4. preparation method according to claim 1, it is characterised in that：
Step 2) described in any one of acrylate in methyl acrylate, ethyl acrylate and butyl acrylate；Institute
Aminostyryl is stated for 3- aminostyryls or 4- aminostyryls.
5. preparation method according to claim 1, it is characterised in that：
Step 2) described in acrylate, styrene and aminostyryl mass ratio be 5~10:1~3:1~3.
6. preparation method according to claim 1, it is characterised in that：
Step 3) described in radical initiator be azo type free radical initiator or peroxy type free radical initiator.
7. preparation method according to claim 1, it is characterised in that：
Step 3) described in the mass ratio of acrylate, the mixed solution of styrene and aminostyryl and radical initiator be
100:0.1~0.5.
8. preparation method according to claim 1, it is characterised in that：
Step 3) described in O/W type emulsions the particle diameter of oil phase drop be 200~2000 μm.
9. a kind of adsorption stuffing of the processing containing aniline waste water, it passes through preparation side according to any one of claim 1 to 8
Method is made.
10. purposes of adsorption stuffing of the processing containing aniline waste water according to claim 9 in being handled containing aniline waste water.
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