CN106076293B - A kind of microballoon and the preparation method and application thereof adsorbing bromophenol blue - Google Patents

A kind of microballoon and the preparation method and application thereof adsorbing bromophenol blue Download PDF

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CN106076293B
CN106076293B CN201610534816.1A CN201610534816A CN106076293B CN 106076293 B CN106076293 B CN 106076293B CN 201610534816 A CN201610534816 A CN 201610534816A CN 106076293 B CN106076293 B CN 106076293B
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microballoon
bromophenol blue
water
polyacrylonitrile
adsorbing
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CN106076293A (en
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许小平
房贺
欧敏锐
祝令辉
谷俊杰
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Fuzhou University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016—Particle form
    • 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
    • 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
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • 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
    • 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
    • C02F2101/36—Organic compounds containing halogen

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention discloses a kind of microballoons and the preparation method and application thereof for adsorbing bromophenol blue, belong to sewage treatment field, the preparation method is that polyacrylonitrile is prepared into microspheroidal, by the way that the itrile group on polyacrylonitrile strand is activated into carboxyl with lye, obtain finished product microballoon, the electronegativity of the meagre profit prepared using this method carboxyl presented in water, the bromophenol blue being dissolved in water can effectively be adsorbed, and it can be by adjusting carboxyl-content in form and polyacrylonitrile of the pH of solution to control bromophenol blue, to which control is to the adsorption effect of bromophenol blue in aqueous solution.Preparation method of the present invention is simple, with liquid convenient separation, is a kind of method with wide application prospect, can satisfy the demand of the sewage treatment of rapid development.

Description

A kind of microballoon and the preparation method and application thereof adsorbing bromophenol blue
Technical field
The present invention relates to the application of sewage treatment field more particularly to lye in modified polymer material, and in particular to A kind of microballoon and the preparation method and application thereof adsorbing bromophenol blue.
Background technique
With the development of the industries such as weaving, leather, plastics, organic dyestuff is widely used, but due to technical Limitation and industry in it is lack of standardization, a large amount of organic dyestuff is discharged into water, becomes one of the major pollutants in water.Have Engine dyeing material is difficult to be biodegradable since its complicated aromatic structure is very firm in water.These dyestuffs not only can be to people Health causes very big harm, while can also seriously affect the ecological environment on periphery.
Ultrafiltration and absorption are the most common two kinds of means of organic dyestuff in processing water.Polyacrylonitrile is excellent physico with its It learns stability and solvent resistance and is widely used in the preparation of ultrafiltration membrane, but cause disengaging time mistake since film is often blocked It is long, separative efficiency decline, and clean to get up to will increase additional cost.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of preparation process is simple, operating condition is mild, Adsorption capacity it is strong for adsorbing the microballoon and preparation method thereof of bromophenol blue in water, the microballoon that is prepared using this method can be with Bromophenol blue is effectively combined on carboxyl by ionic adsorption using the charging property of carboxyl in aqueous solution, maximum can be imitated Remove pollutant to rate.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of method for preparing microsphere adsorbing bromophenol blue comprising following steps:
1) microballoon liquid is prepared: polyacrylonitrile (PAN) powder and dimethyl sulfoxide for being 10-15:85-90 by mass percent (DMSO) solution is uniformly mixed, and heating water bath at 45-50 DEG C, magnetic agitation 3-3.5h obtains microballoon liquid, and the microballoon liquid is Bright yellow solution；
2) it prepares microballoon: above-mentioned microballoon liquid being extracted out from hose with pump, microballoon liquid is flowed out in the form of drop, is used in combination The beaker for filling with water catches drop, and dimethyl sulfoxide dissolves in water at this time, and polyacrylonitrile then sinks to bottom of the beaker in the form of microballoon Portion；
3) modified: the microballoon that above-mentioned steps are obtained is pulled out from water, is dried, and is put into the lye of 1-10mol/L modified 40-180min, polyacrylonitrile microballoon becomes yellow from white at this time；
4) double decomposition: modified microballoon is taken out from lye, is impregnated 1-1.5h into the water, is then put into microballoon Metathesis reaction, reaction time 30-60min are carried out in the hydrochloric acid solution of 0.5-2mol/L；Reaction temperature is 20-40 DEG C, this Shi Weiqiu is again transformed into white by yellow, and microballoon taking-up is placed again into water and impregnates 1-1.5h, removes remaining hydrochloric acid, so It is afterwards that microballoon is dry, obtain the microballoon of absorption bromophenol blue.
The mass percent of the step 1), polyacrylonitrile and dimethyl sulfoxide is 10:90.
The step 3), lye are sodium hydroxide solution or potassium hydroxide solution.
Further, the step 3), lye molar concentration are 1-2mol/L, modification time 40-60min.
The step 4), reaction temperature are preferably 40 DEG C.
The step 4), the molar concentration of hydrochloric acid are 1mol/L.
Water in the step 2) and step 4) is distilled water.
The step 4), the drying are using vacuum freeze drying.
Microballoon of the present invention is used to adsorb the bromophenol blue in water, and concrete application method is, by the pH tune of pending water Section is 4.5-6.5, by microballoon as 30-40min is adsorbed in pending water, the shape of the adjustable bromophenol blue of pH by adjusting water Carboxyl-content in state and polyacrylonitrile, to remove pollutant in maximum efficiency.
Microballoon of the present invention also has certain adsorption capacity to crystal violet, methylene blue.
The invention adopts the above technical scheme, and polyacrylonitrile is prepared into microspheroidal, is made a return journey by the means of physical absorption Organic dyestuff in water removal utilizes carboxyl that is, by being activated the itrile group on polyacrylonitrile strand at carboxyl with sodium hydroxide The electronegativity presented in water, carry out the bromophenol blue in adsorption aqueous solution.Remarkable advantage of the invention is: modification procedure is simple, Lye used can directly be bought；Modification degree is controllable, and modified material adsorption efficiency is high, can be by adjusting pH value control to bromine The adsorbance of phenol indigo plant is a kind of method with wide application prospect, can satisfy the demand of the sewage treatment of rapid development.
Detailed description of the invention
Fig. 1 is the surface infrared spectrum of microsphere modified front and back；A, polyacrylonitrile；B, carboxylation polyacrylonitrile；
Fig. 2 is the electron microscope for preparing microballoon: A, bead interface；B, microsphere surface；C, microballoon cross section.
Specific embodiment
A kind of preparation method for adsorbing bromophenol blue microballoon, comprising the following steps:
1) microballoon liquid is prepared: polyacrylonitrile (PAN) powder and dimethyl sulfoxide for being 10-15:85-90 by mass percent (DMSO) solution is uniformly mixed, and heating water bath at 45-50 DEG C, magnetic agitation 3-3.5h obtains microballoon liquid, and the microballoon liquid is Bright yellow solution；
2) it prepares microballoon: above-mentioned microballoon liquid being extracted out from hose with pump, microballoon liquid is flowed out in the form of drop, is used in combination The beaker for filling with distilled water catches drop, and dimethyl sulfoxide dissolves in water at this time, and polyacrylonitrile then sinks to burning in the form of microballoon Bottom of a cup portion；
3) modified: the microballoon that above-mentioned steps are obtained is pulled out from water, is dried, and the lye (hydroxide of 1-10mol/L is put into Sodium or potassium hydroxide solution) in modified 40-180min, polyacrylonitrile microballoon becomes yellow from white at this time；
4) double decomposition: modified microballoon is taken out from lye (sodium hydroxide solution or potassium hydroxide solution), is put into 1-1.5h is impregnated in distilled water, then microballoon is put into the hydrochloric acid solution of 0.5-2mol/L and carries out metathesis reaction, when reaction Between be 30-60min；Reaction temperature is 20-40 DEG C, and microballoon is again transformed into white by yellow at this time, and microballoon taking-up is put again Enter and impregnate 1-1.5h in distilled water, remove remaining hydrochloric acid, microballoon is then put into drying in vacuum refrigerating machine, obtains absorption bromine The microballoon of phenol indigo plant.
The microballoon is used to adsorb the bromophenol blue in water, and concrete application method is to be adjusted to the pH of pending water 4.5-6.5, by microballoon as adsorbing 30-40min in pending water.
Below in conjunction with specific example, the present invention is further described, but the present invention is not limited only to this.
Embodiment 1
A kind of preparation method for adsorbing bromophenol blue microballoon, comprising the following steps:
1) microballoon liquid is prepared: polyacrylonitrile (PAN) powder and dimethyl sulfoxide (DMSO) for being 10:90 by mass percent Solution is uniformly mixed, heating water bath at 50 DEG C, magnetic agitation 3h, obtains microballoon liquid, and the microballoon liquid is clear yellow solution；
2) it prepares microballoon: above-mentioned microballoon liquid being extracted out from hose with pump, microballoon liquid is flowed out in the form of drop, is used in combination The beaker for filling with distilled water catches drop, and dimethyl sulfoxide dissolves in water at this time, and polyacrylonitrile then sinks to burning in the form of microballoon Bottom of a cup portion；
3) modified: the microballoon that above-mentioned steps are obtained is pulled out from water, is dried, be put into 1mol/L sodium hydroxide or in change Property 40min, polyacrylonitrile microballoon becomes yellow from white at this time；
4) double decomposition: modified microballoon being taken out from sodium hydroxide solution, is put into distilled water and impregnates 1h, then will Microballoon, which is put into the hydrochloric acid solution of 0.5mol/L, carries out metathesis reaction, reaction time 30min；Reaction temperature is 40 DEG C, this Shi Weiqiu is again transformed into white by yellow, and microballoon taking-up is placed again into distilled water and impregnates 1h, removes remaining hydrochloric acid, so Microballoon is put into drying in vacuum refrigerating machine afterwards, obtains the microballoon of absorption bromophenol blue.
The microballoon is used to adsorb the bromophenol blue in water, and concrete application method is to be adjusted to the pH of pending water 5.0, by microballoon as adsorbing 30min in pending water.
Embodiment 2
A kind of preparation method for adsorbing bromophenol blue microballoon, comprising the following steps:
1) microballoon liquid is prepared: polyacrylonitrile (PAN) powder and dimethyl sulfoxide (DMSO) for being 15:85 by mass percent Solution is uniformly mixed, heating water bath at 50 DEG C, magnetic agitation 3.5h, obtains microballoon liquid, and the microballoon liquid is clear yellow solution；
2) it prepares microballoon: above-mentioned microballoon liquid being extracted out from hose with pump, microballoon liquid is flowed out in the form of drop, is used in combination The beaker for filling with distilled water catches drop, and dimethyl sulfoxide dissolves in water at this time, and polyacrylonitrile then sinks to burning in the form of microballoon Bottom of a cup portion；
3) modified: the microballoon that above-mentioned steps are obtained is pulled out from water, is dried, be put into 2mol/L sodium hydroxide or in change Property 60min, polyacrylonitrile microballoon becomes yellow from white at this time；
4) double decomposition: modified microballoon is taken out from sodium hydroxide solution, is put into distilled water and impregnates 1.5h, then Microballoon is put into the hydrochloric acid solution of 2mol/L and carries out metathesis reaction, reaction time 60min；Reaction temperature is 20 DEG C, this Shi Weiqiu is again transformed into white by yellow, and microballoon taking-up is placed again into distilled water and impregnates 1.5h, removes remaining hydrochloric acid, Then microballoon is put into drying in vacuum refrigerating machine, obtains the microballoon of absorption bromophenol blue.
The microballoon is used to adsorb the bromophenol blue in water, and concrete application method is to be adjusted to the pH of pending water 4.5, by microballoon as adsorbing 30min in pending water.
Embodiment 3
A kind of preparation method for adsorbing bromophenol blue microballoon, comprising the following steps:
1) microballoon liquid is prepared: polyacrylonitrile (PAN) powder and dimethyl sulfoxide (DMSO) for being 12:88 by mass percent Solution is uniformly mixed, heating water bath at 50 DEG C, magnetic agitation 3h, obtains microballoon liquid, and the microballoon liquid is clear yellow solution；
2) it prepares microballoon: above-mentioned microballoon liquid being extracted out from hose with pump, microballoon liquid is flowed out in the form of drop, is used in combination The beaker for filling with distilled water catches drop, and dimethyl sulfoxide dissolves in water at this time, and polyacrylonitrile then sinks to burning in the form of microballoon Bottom of a cup portion；
3) modified: the microballoon that above-mentioned steps are obtained is pulled out from water, is dried, and the lye (sodium hydroxide of 10mol/L is put into Or potassium hydroxide solution) in modified 180min, polyacrylonitrile microballoon becomes yellow from white at this time；
4) double decomposition: modified microballoon is taken out from lye (sodium hydroxide solution or potassium hydroxide solution), is put into 1h is impregnated in distilled water, then microballoon is put into the hydrochloric acid solution of 1mol/L and carries out metathesis reaction, and the reaction time is 40min；Reaction temperature is 30 DEG C, and microballoon is again transformed into white by yellow at this time, and microballoon taking-up is placed again into distilled water 1h is impregnated, remaining hydrochloric acid is removed, microballoon is then put into drying in vacuum refrigerating machine, obtains the microballoon of absorption bromophenol blue.
The microballoon is used to adsorb the bromophenol blue in water, and concrete application method is to be adjusted to the pH of pending water 6.5, by microballoon as adsorbing 40min in pending water.
Application examples 1
Microballoon of the invention is applied to the measurement of water adsorption effect:
The 0.03g modified polyacrylonitrile microballoon of 1mol/L sodium hydroxide solution (the preparation method is the same as that of Example 1) is taken, is put Enter 3mL, in the bromophenol blue solution of 1mg/L, takes out bromophenol blue after 30min.Before being adsorbed with measurement of ultraviolet-visible spectrophotometer The absorbance of solution afterwards finds the concentration of absorption front and back according to working curve, then according to formula R=(1-C1/C0) × 100% Calculate adsorption rate (R, adsorption rate；C1The concentration of solution after absorption；C0, the concentration of solution before adsorbing).
The result shows that effectively removing the bromine phenol in solution with polyacrylonitrile microballoon of the sodium hydroxide solution after modified Indigo plant, bromophenol blue solution concentration are reduced to 0.2mg/L, adsorption rate 80% from 1mg/L.
Application examples 2
Influence of the concentration of lye to polyacrylonitrile microballoon adsorption capacity:
Use modified (the same embodiment of preparation method of sodium hydroxide solution of 2mol/L during preparation polyacrylonitrile microballoon instead 1), determining adsorption method is that absorption dyestuff carries out a series of evaluations with bromophenol blue with the method in application examples 1.
The result shows that effectively removing the bromine phenol in solution with polyacrylonitrile microballoon of the sodium hydroxide solution after modified It is blue.Bromophenol blue solution concentration is reduced to 0.14mg/L, adsorption rate 86%, with the raising of concentration of lye, polypropylene from 1mg/L Carboxylated grade increases on nitrile microballoon, and adsorption effect is more excellent.But concentration of lye is excessively high to cause certain damage, concentration to microballoon It does not answer, more than 10mol/L.
Application examples 3
Influence of the modification time to polyacrylonitrile microballoon adsorption capacity:
It is used instead during preparation polyacrylonitrile microballoon and is increased to modification time 1h (the preparation method is the same as that of Example 1), adsorbed Ability measuring method is that absorption dyestuff carries out a series of evaluations with bromophenol blue with the method in application examples 1.
The result shows that effectively removing the bromine phenol in solution with polyacrylonitrile microballoon of the sodium hydroxide solution after modified Indigo plant, bromophenol blue solution concentration are reduced to 0.16mg/L, adsorption rate 84%, with the increase of modification time, polypropylene from 1mg/L Carboxylated grade increases on nitrile microballoon, and adsorption effect is more excellent.But modification time is too long to cause certain damage to microballoon, be modified 3h is not to be exceeded in time.
Application examples 4
Influence of the pH of pending water solution to polyacrylonitrile microballoon adsorption capacity:
The pH of bromophenol blue solution is changed to 7, adsorption capacity measuring method is to inhale with bromophenol blue with the method in application examples 1 Attached dye carries out a series of evaluations.
The result shows that effectively removing the bromine phenol in solution with polyacrylonitrile microballoon of the sodium hydroxide solution after modified Indigo plant, bromophenol blue solution concentration are reduced to 0.93mg/L from 1mg/L, adsorption efficiency 7%, with the increase of solution ph, poly- third Alkene nitrile microballoon reduces the adsorption effect of bromophenol blue.Microballoon has more strict requirements, optimum pH range to absorption environment For 4.5-6.5.Adsorption rate is different under the conditions of different pH, shows higher adsorption rate in acid condition.In pH= Adsorption rate reaches 90% under the conditions of 5.8, for bromophenol blue, Optimal pH 5.4.
Microballoon of the invention is during the preparation process, the step 3), when being improved with lye to microballoon, lye it is dense When degree, modification time and adsorption applications, influence of the pH of bromophenol blue solution to microballoon adsorption capacity is as follows；
Fig. 1 is that the surface composition of microsphere modified front and back analyzes (microsphere surface infrared spectrum): A is polyacrylonitrile；B is carboxylation Polyacrylonitrile；Illustrated by the microsphere surface infrared spectrum of Fig. 1 successfully by part nitrile-group modification on polyacrylonitrile at carboxyl.
Fig. 2 is the electron microscopic morphology analysis of microballoon: A is bead interface, is equivalent to a tunic, and inside is irregular hollow knot Structure；B is microsphere surface, relatively rough；C is microballoon cross section, it is seen that is a kind of hollow morphology for having many channels inside microballoon.

Claims (10)

1. it is a kind of adsorb bromophenol blue method for preparing microsphere, it is characterised in that: itself the following steps are included:
1) it prepares microballoon liquid: polyacrylonitrile and dimethyl sulfoxide that mass percent is 10-15:85-90 being uniformly mixed, 45- Heating water bath at 50 DEG C, magnetic agitation 3-3.5h obtain microballoon liquid；
2) it prepares microballoon: above-mentioned microballoon liquid being extracted out from hose with pump, flows out microballoon liquid in the form of drop, and with filling with The beaker of water catches drop, and dimethyl sulfoxide dissolves in water at this time, and polyacrylonitrile then sinks to beaker bottom in the form of microballoon；
3) modified: the microballoon that above-mentioned steps are obtained is pulled out from water, is dried, and is put into the lye of 1-10mol/L modified 40- 180min,
4) double decomposition: modified microballoon is taken out from lye, is impregnated 1-1.5h into the water, is then put into microballoon Metathesis reaction, reaction time 30-60min are carried out in the hydrochloric acid solution of 0.5-2mol/L；Reaction temperature is 20-40 DEG C, will Microballoon taking-up, which is placed again into water, impregnates 1-1.5h, removes remaining hydrochloric acid, then that microballoon is dry, obtains absorption bromophenol blue Microballoon.
2. a kind of method for preparing microsphere for adsorbing bromophenol blue according to claim 1, it is characterised in that: the step 1), The mass percent of polyacrylonitrile and dimethyl sulfoxide is 10:90.
3. a kind of method for preparing microsphere for adsorbing bromophenol blue according to claim 1, it is characterised in that: the step 3), Lye is sodium hydroxide solution or potassium hydroxide solution.
4. a kind of method for preparing microsphere for adsorbing bromophenol blue according to claim 1, it is characterised in that: the step 3), Lye molar concentration is 1-2mol/L, modification time 40-60min.
5. a kind of method for preparing microsphere for adsorbing bromophenol blue according to claim 1, it is characterised in that: the step 4), Reaction temperature is 40 DEG C.
6. a kind of method for preparing microsphere for adsorbing bromophenol blue according to claim 1, it is characterised in that: the step 4), The molar concentration of hydrochloric acid is 1mol/L.
7. it is according to claim 1 it is a kind of adsorb bromophenol blue method for preparing microsphere, it is characterised in that: the step 2 with Water in step 4) is distilled water.
8. a kind of method for preparing microsphere for adsorbing bromophenol blue according to claim 1, it is characterised in that: the step 4), The drying is using vacuum freeze drying.
9. the microballoon that -8 any preparation methods obtain according to claim 1.
10. the application of microballoon according to claim 9, it is characterised in that: the microballoon is used to adsorb the bromophenol blue in water, Concrete application method is that the pH of pending water is adjusted to 4.5-6.5, microballoon is placed in pending water and adsorbs 30-40min.
CN201610534816.1A 2016-07-08 2016-07-08 A kind of microballoon and the preparation method and application thereof adsorbing bromophenol blue Expired - Fee Related CN106076293B (en)

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