CN106076293A - A kind of microsphere adsorbing bromophenol blue and preparation method and application - Google Patents

A kind of microsphere adsorbing bromophenol blue and preparation method and application Download PDF

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CN106076293A
CN106076293A CN201610534816.1A CN201610534816A CN106076293A CN 106076293 A CN106076293 A CN 106076293A CN 201610534816 A CN201610534816 A CN 201610534816A CN 106076293 A CN106076293 A CN 106076293A
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microsphere
bromophenol blue
water
adsorbing
polyacrylonitrile
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CN106076293B (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)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

The invention discloses a kind of microsphere adsorbing bromophenol blue and preparation method and application, described preparation method is that polyacrylonitrile is prepared as microspheroidal, by the itrile group on polyacrylonitrile strand being activated into carboxyl with alkali liquor, obtain finished product microsphere, utilize the electronegativity presented in water of the slight diarrhea carboxyl that the method prepares, can effectively adsorb the bromophenol blue being dissolved in water, and carboxyl-content in the form of bromophenol blue and polyacrylonitrile can be controlled by the pH of regulation solution, thus control 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 meet the demand of the sewage disposal developed rapidly.

Description

A kind of microsphere adsorbing bromophenol blue and preparation method and application
Technical field
The present invention relates to sewage treatment area, particularly relate to alkali liquor application in modified polymer material, be specifically related to A kind of microsphere adsorbing bromophenol blue and preparation method and application.
Background technology
Along with the development of the industries such as weaving, leather, plastics, organic dyestuff is widely used, but due to technically Restriction and industry in lack of standardization, substantial amounts of organic dyestuff is discharged in water, becomes one of major pollutants in water.Have Organic dye due to the aromatic structure of its complexity in water the most firm, be difficult to be biodegradable.These dyestuffs not only can be to people Health causes the biggest harm, also can have a strong impact on the ecological environment of periphery simultaneously.
Ultrafiltration and absorption are to process two kinds of means that in water, organic dyestuff is the most frequently used.Polyacrylonitrile is excellent physico with it Learn stability and solvent resistance and be widely used in the preparation of ultrafilter membrane, but owing to film is the most blocked and cause disengaging time mistake Long, separation efficiency declines, and cleans to get up to increase extra cost.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of preparation technology is simple, operating condition is gentle, High adsorption capacity for adsorbing microsphere of bromophenol blue and preparation method thereof in water, the microsphere utilizing the method to prepare is permissible Utilize carboxyl charging property in aqueous, by ionic adsorption, bromophenol blue is effectively combined on carboxyl, can maximum imitate Pollutant are removed on rate ground.
To achieve these goals, the present invention adopts the following technical scheme that
A kind of method for preparing microsphere adsorbing bromophenol blue, it comprises the following steps:
1) microsphere liquid is prepared: by polyacrylonitrile (PAN) powder that mass percent is 10-15:85-90 and dimethyl sulfoxide (DMSO) solution mix homogeneously, heating in water bath at 45-50 DEG C, magnetic agitation 3-3.5h, obtain microsphere liquid, described microsphere liquid is Bright yellow solution；
2) prepare microsphere: extracted out from flexible pipe by above-mentioned microsphere liquid pump, make microsphere liquid flow out with the form of drop, and use Drop caught by the beaker filling with water, and during now dimethyl sulfoxide dissolves in water, polyacrylonitrile then sinks at the bottom of beaker with the form of microsphere Portion；
3) modified: microsphere above-mentioned steps obtained is pulled out from water, dries, put in the alkali liquor of 1-10mol/L modified 40-180min, now polyacrylonitrile microballoon is become yellow from white；
4) double decomposition: taken out from alkali liquor by modified microsphere, puts into immersion 1-1.5h in water, is then put into by microsphere Carrying out metathesis reaction in the hydrochloric acid solution of 0.5-2mol/L, the response time is 30-60min；Reaction temperature is 20-40 DEG C, this Shi Weiqiu is again transformed into white by yellow, is taken out by microsphere and is placed again in water soaking 1-1.5h, removes the hydrochloric acid of residual, so After microsphere is dried, obtain adsorb bromophenol blue microsphere.
Described step 1), the mass percent of polyacrylonitrile and dimethyl sulfoxide is 10:90.
Described step 3), alkali liquor is sodium hydroxide solution or potassium hydroxide solution.
Further, described step 3), alkali liquor molar concentration is 1-2mol/L, and modification time is 40-60min.
Described step 4), reaction temperature is preferably 40 DEG C.
Described step 4), the molar concentration of hydrochloric acid is 1mol/L.
Described step 2) with step 4) in water be distilled water.
Described step 4), described be dried into use vacuum lyophilization.
Microsphere of the present invention is for adsorbing the bromophenol blue in water, and its concrete application process is, is adjusted by the pH of pending water Joint is 4.5-6.5, by microsphere as adsorbing 30-40min in pending water, can be regulated the shape of bromophenol blue by the pH of regulation water Carboxyl-content in state and polyacrylonitrile, thus remove pollutant in maximum efficiency.
Microsphere of the present invention also has certain absorbability to crystal violet, methylene blue.
The present invention uses above technical scheme, and polyacrylonitrile is prepared as microspheroidal, is made a return journey by the means of physical absorption Except the organic dyestuff in water, i.e. by the itrile group on polyacrylonitrile strand being activated into carboxyl with sodium hydroxide, utilize carboxyl The electronegativity presented in water, carry out the bromophenol blue in adsorption aqueous solution.The remarkable advantage of the present invention is: modification procedure is simple, Alkali liquor used can directly be bought；Modified degree is controlled, and modified material adsorption efficiency is high, can be controlled bromine by regulation pH value The adsorbance that phenol is blue, is a kind of method with wide application prospect, can meet the demand of the sewage disposal developed rapidly.
Accompanying drawing explanation
Fig. 1 be microsphere modified before and after surface infrared spectrum；A, polyacrylonitrile；B, carboxylation polyacrylonitrile；
Fig. 2 is the Electronic Speculum figure preparing microsphere: A, bead interface；B, microsphere surface；C, microsphere cross section.
Detailed description of the invention
A kind of preparation method adsorbing bromophenol blue microsphere, comprises the following steps:
1) microsphere liquid is prepared: by polyacrylonitrile (PAN) powder that mass percent is 10-15:85-90 and dimethyl sulfoxide (DMSO) solution mix homogeneously, heating in water bath at 45-50 DEG C, magnetic agitation 3-3.5h, obtain microsphere liquid, described microsphere liquid is Bright yellow solution；
2) prepare microsphere: extracted out from flexible pipe by above-mentioned microsphere liquid pump, make microsphere liquid flow out with the form of drop, and use Drop caught by the beaker filling with distilled water, and during now dimethyl sulfoxide dissolves in water, polyacrylonitrile then sinks to burn with the form of microsphere Bottom Bei；
3) modified: microsphere above-mentioned steps obtained is pulled out from water, dries, and puts into the alkali liquor (hydroxide of 1-10mol/L Sodium or potassium hydroxide solution) in modified 40-180min, now polyacrylonitrile microballoon is become yellow from white；
4) double decomposition: modified microsphere is taken out from alkali liquor (sodium hydroxide solution or potassium hydroxide solution), puts into Distilled water soaks 1-1.5h, then microsphere is put into and the hydrochloric acid solution of 0.5-2mol/L carries out metathesis reaction, during reaction Between be 30-60min；Reaction temperature is 20-40 DEG C, and now microsphere is again transformed into white by yellow, is taken out by microsphere and again puts Enter immersion 1-1.5h in distilled water, remove the hydrochloric acid of residual, then microsphere is put in vacuum refrigerating machine and be dried, obtain adsorbing bromine The microsphere that phenol is blue.
Described microsphere is for adsorbing the bromophenol blue in water, and its concrete application process is, by the pH regulator of pending water is 4.5-6.5, by microsphere as adsorbing 30-40min in pending water.
Below in conjunction with instantiation, further describe the present invention, but the present invention is not limited only to this.
Embodiment 1
A kind of preparation method adsorbing bromophenol blue microsphere, comprises the following steps:
1) microsphere liquid is prepared: by polyacrylonitrile (PAN) powder that mass percent is 10:90 and dimethyl sulfoxide (DMSO) Solution mix homogeneously, heating in water bath at 50 DEG C, magnetic agitation 3h, obtain microsphere liquid, described microsphere liquid is clear yellow solution；
2) prepare microsphere: extracted out from flexible pipe by above-mentioned microsphere liquid pump, make microsphere liquid flow out with the form of drop, and use Drop caught by the beaker filling with distilled water, and during now dimethyl sulfoxide dissolves in water, polyacrylonitrile then sinks to burn with the form of microsphere Bottom Bei；
3) modified: microsphere above-mentioned steps obtained is pulled out from water, dries, put into 1mol/L sodium hydroxide or in change Property 40min, now polyacrylonitrile microballoon is become yellow from white；
4) double decomposition: taken out from sodium hydroxide solution by modified microsphere, puts into immersion 1h in distilled water, then will Microsphere is put in the hydrochloric acid solution of 0.5mol/L and is carried out metathesis reaction, and the response time is 30min；Reaction temperature is 40 DEG C, this Shi Weiqiu is again transformed into white by yellow, is taken out by microsphere and is placed again in distilled water soaking 1h, removes the hydrochloric acid of residual, so After microsphere put in vacuum refrigerating machine and is dried, obtain adsorbing the microsphere of bromophenol blue.
Described microsphere is for adsorbing the bromophenol blue in water, and its concrete application process is, by the pH regulator of pending water is 5.0, by microsphere as pending water adsorbs 30min.
Embodiment 2
A kind of preparation method adsorbing bromophenol blue microsphere, comprises the following steps:
1) microsphere liquid is prepared: by polyacrylonitrile (PAN) powder that mass percent is 15:85 and dimethyl sulfoxide (DMSO) Solution mix homogeneously, heating in water bath at 50 DEG C, magnetic agitation 3.5h, obtain microsphere liquid, described microsphere liquid is clear yellow solution；
2) prepare microsphere: extracted out from flexible pipe by above-mentioned microsphere liquid pump, make microsphere liquid flow out with the form of drop, and use Drop caught by the beaker filling with distilled water, and during now dimethyl sulfoxide dissolves in water, polyacrylonitrile then sinks to burn with the form of microsphere Bottom Bei；
3) modified: microsphere above-mentioned steps obtained is pulled out from water, dries, put into 2mol/L sodium hydroxide or in change Property 60min, now polyacrylonitrile microballoon is become yellow from white；
4) double decomposition: taken out from sodium hydroxide solution by modified microsphere, puts into immersion 1.5h in distilled water, then Being put into by microsphere and carry out metathesis reaction in the hydrochloric acid solution of 2mol/L, the response time is 60min；Reaction temperature is 20 DEG C, this Shi Weiqiu is again transformed into white by yellow, is taken out by microsphere and is placed again in distilled water soaking 1.5h, removes the hydrochloric acid of residual, Then microsphere is put in vacuum refrigerating machine and be dried, obtain adsorbing the microsphere of bromophenol blue.
Described microsphere is for adsorbing the bromophenol blue in water, and its concrete application process is, by the pH regulator of pending water is 4.5, by microsphere as pending water adsorbs 30min.
Embodiment 3
A kind of preparation method adsorbing bromophenol blue microsphere, comprises the following steps:
1) microsphere liquid is prepared: by polyacrylonitrile (PAN) powder that mass percent is 12:88 and dimethyl sulfoxide (DMSO) Solution mix homogeneously, heating in water bath at 50 DEG C, magnetic agitation 3h, obtain microsphere liquid, described microsphere liquid is clear yellow solution；
2) prepare microsphere: extracted out from flexible pipe by above-mentioned microsphere liquid pump, make microsphere liquid flow out with the form of drop, and use Drop caught by the beaker filling with distilled water, and during now dimethyl sulfoxide dissolves in water, polyacrylonitrile then sinks to burn with the form of microsphere Bottom Bei；
3) modified: microsphere above-mentioned steps obtained is pulled out from water, dries, and puts into the alkali liquor (sodium hydroxide of 10mol/L Or potassium hydroxide solution) in modified 180min, now polyacrylonitrile microballoon is become yellow from white；
4) double decomposition: modified microsphere is taken out from alkali liquor (sodium hydroxide solution or potassium hydroxide solution), puts into Soaking 1h in distilled water, then put into by microsphere and carry out metathesis reaction in the hydrochloric acid solution of 1mol/L, the response time is 40min；Reaction temperature is 30 DEG C, and now microsphere is again transformed into white by yellow, is taken out by microsphere and is placed again in distilled water Soak 1h, remove the hydrochloric acid of residual, then microsphere is put in vacuum refrigerating machine and be dried, obtain adsorbing the microsphere of bromophenol blue.
Described microsphere is for adsorbing the bromophenol blue in water, and its concrete application process is, by the pH regulator of pending water is 6.5, by microsphere as pending water adsorbs 40min.
Application examples 1
The microsphere of the present invention is applied to the mensuration of water adsorption effect:
Take the modified polyacrylonitrile microballoon of 0.03g 1mol/L sodium hydroxide solution (preparation method is with embodiment 1), put Enter in the bromophenol blue solution of 3mL, 1mg/L, after 30min, bromophenol blue is taken out.Before adsorbing with measurement of ultraviolet-visible spectrophotometer The absorbance of rear solution, finds the concentration before and after absorption 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 absorption).
Result shows, effectively removes the bromine phenol in solution by the polyacrylonitrile microballoon after sodium hydroxide solution modification Indigo plant, bromophenol blue solution concentration is reduced to 0.2mg/L from 1mg/L, and adsorption rate is 80%.
Application examples 2
The concentration of lye impact on polyacrylonitrile microballoon absorbability:
Modified (the same embodiment of preparation method of sodium hydroxide solution of 2mol/L is used instead during preparation polyacrylonitrile microballoon 1), determining adsorption method, with the method in application examples 1, carries out a series of evaluation with bromophenol blue for absorbing dye.
Result shows, effectively removes the bromine phenol in solution by the polyacrylonitrile microballoon after sodium hydroxide solution modification Blue.Bromophenol blue solution concentration is reduced to 0.14mg/L from 1mg/L, and adsorption rate is 86%, along with the raising of concentration of lye, polypropylene On nitrile microsphere, carboxylated grade increases, and adsorption effect is more excellent.But microsphere is caused certain infringement, concentration by the too high meeting of concentration of lye Do not answer, more than 10mol/L.
Application examples 3
The modification time impact on polyacrylonitrile microballoon absorbability:
Use instead during preparation polyacrylonitrile microballoon and modification time is brought up to 1h (preparation method is with embodiment 1), absorption Ability assay method, with the method in application examples 1, carries out a series of evaluation with bromophenol blue for absorbing dye.
Result shows, effectively removes the bromine phenol in solution by the polyacrylonitrile microballoon after sodium hydroxide solution modification Indigo plant, bromophenol blue solution concentration is reduced to 0.16mg/L from 1mg/L, and adsorption rate is 84%, along with the increase of modification time, polypropylene On nitrile microsphere, carboxylated grade increases, and adsorption effect is more excellent.But microsphere is caused certain infringement by the long meeting of modification time, modified Time is not to be exceeded 3h.
Application examples 4
The pH of the pending aqueous solution impact on polyacrylonitrile microballoon absorbability:
The pH of bromophenol blue solution changes into 7, and absorbability assay method is with the method in application examples 1, with bromophenol blue for inhaling Attached dye carries out a series of evaluation.
Result shows, effectively removes the bromine phenol in solution by the polyacrylonitrile microballoon after sodium hydroxide solution modification Indigo plant, bromophenol blue solution concentration is reduced to 0.93mg/L from 1mg/L, and adsorption efficiency is 7%, along with the increase of solution ph, poly-third The adsorption effect of bromophenol blue is reduced by alkene nitrile microsphere.Microsphere has more strict requirements, optimum pH scope 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.At pH= Under the conditions of 5.8, adsorption rate reaches 90%, and from the point of view of bromophenol blue, Optimal pH is 5.4.
The microsphere of the present invention in preparation process, described step 3), when microsphere being improved with alkali liquor, alkali liquor dense When degree, modification time and adsorption applications, the pH of bromophenol blue solution is as follows on the impact of microsphere absorbability；
Fig. 1 be microsphere modified before and after surface composition analysis (microsphere surface infrared spectrum): A is polyacrylonitrile；B is carboxylation Polyacrylonitrile；Illustrated the most successfully polyacrylonitrile upper part nitrile-group modification to be become carboxyl by the microsphere surface infrared spectrum of Fig. 1.
Fig. 2 is the electron microscopic morphology analysis of microsphere: A is bead interface, is equivalent to a tunic, and inside is irregular hollow knot Structure；B is microsphere surface, relatively rough；C is microsphere cross section, it is seen that be that one has the most multichannel hollow morphology inside microsphere.

Claims (10)

1. the method for preparing microsphere adsorbing bromophenol blue, it is characterised in that: it comprises the following steps:
1) microsphere liquid is prepared: by polyacrylonitrile that mass percent is 10-15:85-90 and dimethyl sulfoxide mix homogeneously, 45- Heating in water bath at 50 DEG C, magnetic agitation 3-3.5h, obtain microsphere liquid；
2) prepare microsphere: extracted out from flexible pipe by above-mentioned microsphere liquid pump, make microsphere liquid flow out with the form of drop, and with containing Drop caught by the beaker of full water, and during now dimethyl sulfoxide dissolves in water, polyacrylonitrile then sinks to beaker bottom with the form of microsphere；
3) modified: microsphere above-mentioned steps obtained is pulled out from water, dries, put into modified 40-in the alkali liquor of 1-10mol/L 180min,
4) double decomposition: taken out from alkali liquor by modified microsphere, puts into immersion 1-1.5h in water, is then put into by microsphere Carrying out metathesis reaction in the hydrochloric acid solution of 0.5-2mol/L, the response time is 30-60min；Reaction temperature is 20-40 DEG C, will Microsphere takes out and is placed again in water soaking 1-1.5h, removes the hydrochloric acid of residual, is then dried by microsphere, obtains adsorbing bromophenol blue Microsphere.
A kind of method for preparing microsphere adsorbing bromophenol blue the most according to claim 1, it is characterised in that: described step 1), The mass percent of polyacrylonitrile and dimethyl sulfoxide is 10:90.
A kind of method for preparing microsphere adsorbing bromophenol blue the most according to claim 1, it is characterised in that: described step 3), Alkali liquor is sodium hydroxide solution or potassium hydroxide solution.
A kind of method for preparing microsphere adsorbing bromophenol blue the most according to claim 1, it is characterised in that: described step 3), Alkali liquor molar concentration is 1-2mol/L, and modification time is 40-60min.
A kind of method for preparing microsphere adsorbing bromophenol blue the most according to claim 1, it is characterised in that: described step 4), Reaction temperature is 40 DEG C.
A kind of method for preparing microsphere adsorbing bromophenol blue the most according to claim 1, it is characterised in that: described step 4), The molar concentration of hydrochloric acid is 1mol/L.
A kind of method for preparing microsphere adsorbing bromophenol blue the most according to claim 1, it is characterised in that: described step 2) with Water in step 4) is distilled water.
A kind of method for preparing microsphere adsorbing bromophenol blue the most according to claim 1, it is characterised in that: described step 4), Described be dried into use vacuum lyophilization.
9. the microsphere obtained according to the arbitrary preparation method of claim 1-8.
The application of microsphere the most according to claim 9, it is characterised in that: described microsphere is used for adsorbing the bromophenol blue in water, its Concrete application process is to be 4.5-6.5 by the pH regulator of pending water, by microsphere as adsorbing 30-40min in pending water.
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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Publication number Priority date Publication date Assignee Title
CN109704299A (en) * 2019-02-28 2019-05-03 武汉工程大学 The method that phosphate discharge liquid prepares potassium dihydrogen phosphate

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109704299A (en) * 2019-02-28 2019-05-03 武汉工程大学 The method that phosphate discharge liquid prepares potassium dihydrogen phosphate

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